1601 - Indus Chem Lab Manual

Department of Chemical Engineering
Industrial Chemistry
(CHEM 85)
Laboratory Manual
Compiled by
Chemical Engineering Department
First Edition
2015
PREFACE
The purpose of this laboratory manual is to serve as instructional book for students,
instructors, and laboratory technician to assist in performing and understanding the
experiments in Industrial Chemistry.
GENERAL INFORMATION ABOUT

INDUSTRIAL CHEMISTRY COURSE
RATIONALE
As future chemical engineers, ChE students must be equipped with in-depth knowledge
and appropriate skills necessary for the practice of the profession particularly in the
industry. To that end, each student are expected to successfully (1) identify the major
manufacturing steps necessary for the production of goods from raw materials, (2)
explain underlying chemical reactions involved in industrial processes, and (3) develop a
positive attitude towards research for lifelong learning.
COURSE DESCRIPTION
This course equips focuses on the (1) basic raw materials, (2) reaction mechanisms
involved, and (3) major manufacturing steps used in the industrial production of
consumer products such as: oils and fats, flavors and fragrances, sugar and salt refining,
fermentation, soap and detergents, hydrogen peroxide and inorganic hydrogen peroxy
compounds, industrial acids and bases, pulp and paper, polymers, petrochemicals, paints,
pigments and industrial coatings, catalysis and its industrial application.
COURSE LEARNING OUTCOMES (CLOS)
Upon successful completion of the course, the students should be able to attain the
following learning outcomes.
CLO1. Identify the major manufacturing steps necessary for the production of goods from
raw materials.
CLO2. Explain underlying chemical reactions involved in industrial processes.
CLO3. Develop a positive attitude towards researchexecute laboratory procedures,
giving considerations on safety.
CLO4. Convey ideas effectively through written laboratory reports.
OPPORTUNITIES TO DEVELOP LIFELONG LEARNING SKILLS
1. Students may visit online websites of different chemical plants and look for
simulations or videos of their actual processes.
2. Students may also take the summer immersion course and explore other processes that
would yield similar products compared to those discussed in class.
COURSE OUTLINE (Adapted from CMO 23, S. 2008, Annex III)
Week
Topic/subtopic learning
outcomes
Topics/subtopics
i.
Wk.1-2
(June 9,
16 and
19)
Wk.3
Introduction to Industrial
Chemistry Course
a. Course syllabus
b. Overview of topics
ii.
Chemistry of Oils, Fats
i.
iii.
Short revisit of needed

basic chemistry topics
Gain insight on course
coverage and
requirements
Be familiar with the
history of industrial
chemistry
Draw molecular structure
Assessment
Task(s)
Teaching and
Learning
Activities (TLA)
Scoring Tool
Lec1: Discussion
Aptitude test
Problem
Lab1: Laboratory
Orientation
Rubric C & D
Lec2: Lecture,
Test Score
(June 23
and 26)
and Wax Processing

a. Similarities and
differences in
chemical structure
b. Production
processes and
chemical reactions
involved
ii.
iii.
of fats, oils and waxes

Write chemical reactions
involving fats, oils and
waxes
Define manufacturing
processes for fats, oils
and waxes
Problem-based
Learning
Pre-lab quiz
Lab Report
Lab2: Coconut
Extraction and Oil
Refining
Quiz score,
Rubric C & D
Objective-type
test and
problem
solving
Lec3: Case Study/

Video clips on oils
and wax
processing
Test Score
Pre-lab quiz
Lab Report
Lab3: Extraction
of Essential Oils
Quiz score,
Rubric C & D
Concept
mapping and
Problem
solving
Lec4: Lecture,
Video
presentation,
Group discussion
Test Score
Pre-lab quiz
Lab Report
Lab4: Production
of laundry or Bath
soap
Quiz score,
Rubric C & D
Lec5: Lecture,
Video presentation
Test Score
Pre-lab quiz
Lab Report
Lab5: Refining of
sugar and salt
Quiz score,
Rubric C & D
Problem set
Lec6: Lecture,
Problem solving
Test Score
Lab6: Production
of Paper
Quiz score,
Rubric C & D
Lec7: Discussion
Rubric B
Lab7:
Fermentation:
Wine
Quiz score,
Rubric C & D
Problem set
Lec8: Problembased learning
Test Score
Pre-lab quiz
Lab Report
Lab8:
Fermentation:
Cheese
Quiz score,
Rubric C & D
Discussion
paper
Lec9: Discussion,
Role play
Rubric B
Pre-lab quiz
Lab9:
Fermentation:
Quiz score,
Rubric C & D
i.
Wk.4-5
(July 3, 7
and 10)
Chemistry of Flavours
and Fragrances
a. Chemical
composition of
Essential Oils
b. Methods of
extraction
Chemistry of Surfactants
and the Manufacture of
Soap and Detergents
Wk.6-7
(July 14,
17, and
21)
Wk.8
(July 28)
Wk.9
(Aug. 4
and 7)
10
Wk.11
(Aug.18)
Wk.12
(Aug.25)
Wk.13
(Sept.1
and 4)
LONG EXAM 1
(Prelim)
Chemistry of Saccharides
a. Recovery of Sugar
from Principal Sources
b. Refining of Sugar
Pulp and Paper
a. Major Sources of
Pulp
b. Pulping Methods
c. Paper Production
Identify the major

components of essential
oils
ii. Write chemical reactions
involving essential oils
iii. Define manufacturing
processes for flavors and
fragrances
iv. Define saponification
v. Differentiate soaps from
detergents in terms of
their composition and
structure
i. Define sugar
ii. Draw the molecular
structure of saccharides
and basic chemical
reactions involved
iii. Describe the processes
involved in sugar
refining
solving
Define pulp
Explain different pulping
methods employed in
industry
iii. Describe paper
production steps
i.
ii.
Fermentation Processes
i.
and their Application
ii.
a. Fermented food and
beverage
b. Industrial chemicals
iii.
and pharmaceuticals
MIDTERM EXAMINATION
Define fermentation
Draw chemical reactions
involved in alcoholic and
lactic acid fermentation
Describe upstream and
downstream processes
Hydrogen Peroxide and

Inorganic Peroxy Cpds
Pre-lab quiz
Lab Report
Discussion
paper
Midterm Processing and

Evaluation of Student
Progress
Catalysts and Catalysis
a. Homogeneous
Catalysis
b. Heterogeneous
Catalysis
c. Application and
Mechanism
Problem
solving
Pre-lab quiz
Lab Report
Define catalysts and
catalysis
ii. Differentiate
homogeneous from
heterogeneous catalysts
iii. Write kinetic expressions
for catalyzed reactions
i. Identify hydrogen
proxide and peroxy
compound derivatives
and their uses
ii. Draw chemical structure
i.
and the reactions

involved
Wk.14
(Sept.8
and 11)
Wk.1516
(Sept. 15,
18 and
22)
Wk.1617
(Sept. 25,
29 and
Oct.2)
18
Industrial Acids and

Bases
a. Common names of
acids and bases
b. Raw materials and
reaction pathways
for production
LONG EXAM
(Semi-Final)
Petrochemicals
a. Petroleum refining
and production of
petrochemicals
b. Groups of
Petrochemicals:
Olefins, Aromatics
and Synthesis Gas
c. Petrochemical
products
Polymer Chemistry
a. Kinds of Polymers:
Natural and Synthetic
b. Polymerization and
Co-polymerization
Reactions
c. Synthetic Polymers:
Plastics and Fibers
Paints, Pigments and
Industrial Coatings
FINAL EXAMINATION
Lab Report
Cheese
Rubric B
i.
ii.
i.
ii.
Determine common
names of acids and bases
Describe chemical
reactions involving acids
and bases
Define petrochemicals
in contrast with
oleochemicals
Describe petroleum
refining processes and
the chemical pathways
for production of
petrochemicals
Define polymer
Classify polymers in
terms of their origin (i.e.
natural vs. synthetic) and
action under heat and
pressure (i.e.
thermoplastic vs
thermosets)
iii. Describe polymerization
reaction
Short
Discussion
Paper
Lec10: Discussion,
Search work
Rubric C & D
Lab10: Plant visit/

Wine
Quality Check
Problem
solving
Lab Report
Lec11: Discussion,
Problem solving
Test Score
Lab11: Plant visit/

Wine
Quality Check
Rubric C & D
i.
ii.
LIST OF RESOURCES
Printed Learning Resources
Textbook:
1. Handbook of Industrial
Chemistry Organic Chemicals,
1st edition by M. F. Ali, B.M.
Ali, J. G. Speight, McGraw-Hill,
2005.
References:
1. Elementary Principles of
Chemical Processes, 3rd ed. by
Richard M. Felder and Ronald
W. Rousseau. John-Wiley and
sons, Inc., 2000.
2. Shreves Chemical Process
Industries, 5th ed. by George T.
Austin. McGraw-Hill, 1984.
COURSE REQUIREMENTS
ConceptMapping
Lec12: Discussion
Lab12: Group
presentation:
Laboratory Results
Rubric A
Web and Other Learning Resources

1. XU ONLINE LIBRARY - can be accessed directly at
our class e-learn site (http://elearn.xu.edu.ph)
2. Youtube: How Its Made Channel,
https://www.youtube.com/channel/UCjHsPBHX1NNb
IqTy4eXVTig
3. DOC BROWN'S CHEMISTRY REVISION notes for
GCSE/IGCSE/O level science students, ~US grades 8,
9, 10 http://www.docbrown.info/page10/page10.htm
4. Michael P. Rosynek, Chemistry 470 - "Industrial
Chemistry" Lecture Notes Spring Semester 2012
https://www.chem.tamu.edu/class/majors/chem470/No
tes.html
5. Industrial Chemistry, Technical Chemistry
http://www.internetchemistry.com/chemistry/industrial
-chemistry.htm
6. Plant/SME visits
Class standing requirements (short quizzes, seatworks, assignments and oral

presentations, group participation and evaluation)
Seatworks and short quizzes are unannounced and are usually given at the start or near
the end of the lecture period. Group problem sets are to be solved through team effort
to maximize peer tutoring and cooperative learning. Each student will be given an
opportunity to make a report on a topic. Each PpT presentation is given a maximum of
10MINUTES. Delivery of presentations is evaluated based on rubric A.
Laboratory Reports Each group is required to submit a single report for each exercise.
These reports will be evaluated based on Rubric B (See Section H) and the format may
be downloaded from the course e-learn account. Reports must be submitted a week
after the exercise is completed. A group is only allowed three days delay in the
submission of reports, after which the reports will no longer be accepted and the group
will receive a grade of zero.
Group Work Participation The members of the group are required to rate each other
on their collaboration in the performance of the activities using the peer evaluation
rubric.
Long tests Examinations covering one (or several) chapters discussed during the
lecture sessions. This type of assessment is announced.
Midterm and Final examination A comprehensive examination covering several
topics discussed. Type of examination is generally computational (problem solving
type) but maybe mixed with objective-type questions (multiple choices, T/F, matching
type, etc). Each student must bring to class his/her own calculator. Borrowing of
calculator during exams and quizzes is NOT ALLOWED.
Plant visit The class can be scheduled to go to chemical processing plants and other
relevant establishments and businesses within the locality relating to a particular
chemical industry. Discussion of the concepts and principles of relevant chemical
process industries will be accomplished during the scheduled lecture hours.
GRADING SYSTEM
A. Midterm grade (MTG)
Prelim Exam/Output
Midterm Exam/Outputs
Class Standing component:
Average of seatworks
Average of quizzes
Average of class participation (board

works and oral presentation)
Average of homeworks and projects

B. Final Grade (FG)
Semi-final Exam/Output
Final Exam (comprehensive in coverage)
Class Standing component:
Average of seatworks
SLMIS code
% in
MTG
% in
FG
PE
ME
20.00
30.00
7.00
10.50
SW-M
QZ-M
CP-M
PRJ-M
10.00
10.00
10.00
20.00
3.50
3.50
3.50
7.00
SE
FE
---
7.00
30.00
SW-F
--
5.00
Grade conversion table

Numerical
grade
92 100
85 91.99
76 84.99
68 75.99
60 67.99
Below 60
Letter
grade
equivale
nt
Description
A
AB
BC
F
Excellent
Very Good
Good
Satisfactory
Passed
Failed
*INC grade is released if a major

requirement is not yet accomplished by
the student AND there is a likely chance
to pass even if the grade for the said
major requirement is assumed at
Average of quizzes
Average of class participation (board
works and oral presentation)
Average of homeworks and projects

TOTAL
QZ-F
CP-F
PRJ-F
----
5.00
5.00
13.00
100.00
100.00
minimum. INC grades are to be

complied with within 1 month from the
start of the next school term (semester or
summer)
ASSESSMENT RUBRICS
Rubric A: Student Presentation (adapted from http://www.ncsu.edu/midlink/rub.pres.html)
1
Audience cannot
understand
presentation because
there is no sequence
of information.
Student does not have
grasp of information;
student cannot answer
questions about
subject.
2
Audience has difficulty
following presentation
because student jumps
around.
3
Student presents
information in logical
sequence which
audience can follow.
Student is
uncomfortable with
information and is able
to answer only
rudimentary questions.
Student is at ease with

expected answers to all
questions, but fails to
elaborate.
Graphics
Student uses
superfluous graphics
or no graphics
Student's graphics
relate to text and
presentation.
Mechanics
Student's presentation
has four or more
spelling errors and/or
grammatical errors.
Student reads all of
report with no eye
contact.
Student occasionally
uses graphics that rarely
support text and
presentation.
Presentation has three
misspellings and/or
grammatical errors.
Organization
Subject
Knowledge
Eye Contact
Elocution
Student mumbles,
incorrectly
pronounces terms,
and speaks too quietly
for students in the
back of class to hear.
Student occasionally
uses eye contact, but
still reads most of
report.
Student's voice is low.
Student incorrectly
pronounces terms.
Audience members have
difficulty hearing
presentation.
Presentation has no
more than two
misspellings and/or
grammatical errors.
Student maintains eye
contact most of the
time but frequently
returns to notes.
Student's voice is clear.
Student pronounces
most words correctly.
Most audience
members can hear
presentation.
4
Student presents
information in logical,
interesting sequence
which audience can
follow.
Student demonstrates full
knowledge (more than
required) by answering
all class questions with
explanations and
elaboration.
Student's graphics
explain and reinforce
screen text and
presentation.
Presentation has no
misspellings or
grammatical errors.
Total
Student maintains eye

contact with audience,
seldom returning to
notes.
Student uses a clear voice
and correct, precise
pronunciation of terms so
that all audience
members can hear
presentation.
Total Points:
Rubric B: Written Report (adapted from http://www.sdst.org/shs/library/resrub.html)

Thesis/Problem/Question
4
Student(s) posed a thoughtful,

creative question that
engaged them in challenging
or provocative research. The
question breaks new ground
or contributes to knowledge
in a focused, specific area.
Student(s) posed a focused

question involving them in
challenging research.
Student(s) constructed a
question that lends itself to
readily available answers
Student(s) relied on teachergenerated questions or
Information
Seeking/Selecting
and Evaluating
Student(s) gathered
information from a
variety of quality
electronic and print
sources, including
appropriate licensed
databases. Sources
are relevant,
balanced and include
critical readings
relating to the thesis
or problem. Primary
sources were
included (if
appropriate).
Student(s) gathered
information from a
variety of relevant
sources--print and
electronic
Student(s) gathered
information from a
limited range of
sources and
displayed minimal
effort in selecting
quality resources
Student(s) gathered
information that
Analysis
Student(s)
carefully analyzed
the information
collected and
drew appropriate
and inventive
conclusions
supported by
evidence. Voice
of the student
writer is evident.
Student (s)
product shows
good effort was
made in analyzing
the evidence
collected
Student(s)
conclusions could
be supported by
stronger evidence.
Level of analysis
could have been
deeper.
Student(s)
conclusions
Synthesis
Documentation
Product/Process
Student(s)
developed
appropriate
structure for
communicating
product,
incorporating
variety of quality
sources.
Information is
logically and
creatively
organized with
smooth
transitions.
Student(s)
logically
organized the
product and made
good connections
among ideas
Student(s)
documented all
sources, including
visuals, sounds, and
animations. Sources
are properly cited,
both in-text/inproduct and on
Works-Cited/WorksConsulted
pages/slides.
Documentation is
error-free.
Student(s) effectively
and creatively used
appropriate
communication tools to
convey their
conclusions and
demonstrated thorough,
effective research
techniques. Product
displays creativity and
originality.
Student(s)
documented sources
with some care,
Sources are cited,
both in-text/inproduct and on
Works-Cited/WorksConsulted
pages/slides. Few
errors noted.
Student(s) need to
use greater care in
documenting
sources.
Documentation was
poorly constructed or
absent.
Student(s) clearly
plagiarized materials.
Student(s) effectively
communicated the
results of research to
the audience.
Student(s) could
have put greater
effort into
organizing the
product
Student(s) work is
not logically or
Student(s) need to
work on
communicating more
effectively
Student(s) showed little

evidence of thoughtful
developed a question
requiring little creative
thought.
lacked relevance,
quality, depth and
balance.
simply involved
restating
information.
Conclusions were
not supported by
evidence.
effectively
structured.
research. Product does

not effectively
communicate research
findings.
Rubric C: Laboratory Report

(adapted from http://www.ncsu.edu/labwrite/instructors/excelsheets.htm#rubric)
Poor
0
Section Points
5
Title
5
Describes lab content concisely, adequately, appropriately
5
Abstract
5
Conveys a sense of the full report concisely and effectively
20
Introduction
3
Successfully establishes the scientific concept of the lab
10
Effectively presents the objectives and purpose of the lab
7
States hypothesis and provides logical reasoning for it
15
Methods
15
Gives enough details to allow for replication of procedure
15
Results
3
Opens with effective statement of overall findings
2
Presents visuals clearly and accurately
5
Presents verbal findings clearly and with sufficient support
5
Successfully integrates verbal and visual representations
15
Discussion
3
Opens with effective statement of support of hypothesis
2
Backs up statement with reference to appropriate findings
5
Provides sufficient and logical explanation for the statement
5
Sufficiently addresses other issues pertinent to lab
10
Conclusion
10
Convincingly describes what has been learned in the lab
5
Presentation
1
Citations and references adhere to proper format
2
Format of tables and figures is correct
1
Report is written in scientific style: clear and to the point
1
Grammar and spelling are correct
10
Overall aims of the report: the student...
3
Has successfully learned what the lab is designed to teach
3
Demonstrates clear and thoughtful scientific inquiry
4
Accurately measures and analyzes data for lab findings
0.25
Average
0.5
0.75
Excellent
1
x
Total Points Earned
Rubric D: Self and Peer Performance Evaluation (during Laboratory)

For each member in the group, evaluate* their effectiveness in the following categories.
Total the points on the right.
Contribution:
Provided
useful ideas
and relevant
information.
Working
with Others:
Listened,
shared, and
worked well
with peers.
Focus:
Stayed
focused on
the task and
what needed
to be done.
Responsibility:
Completes the
assigned task
on time.
3 2 1 0
3 2 1 0
3 2 1 0
3 2 1 0
1.
3 2 1 0
3 2 1 0
3 2 1 0
3 2 1 0
2.
3 2 1 0
3 2 1 0
3 2 1 0
3 2 1 0
Group
Member
Name
TOTAL
POINTS
EARNED
Self-Evaluation
Peer Evaluation
*Rate using the following scale: 3 Excellent, 2 Good, 1 Fair, and 0 Poor/Lacking.
POLICIES
Attendance
Attendance sheets will be passed around and the student is responsible to sign to prove
his presence for that session. This is to monitor whether absences incurred by the
student is still within the allowed number of absences for a course stipulated in the
Student Handbook. The only valid excuses for missing exam are illness requiring
Points
Earned
medical care or a personal/family emergency of a serious nature. For such, valid medical
certificate and parents/guardians letter will be required and subjected to verification.
Cooperative Learning
The goal is to have everyone learn more than they would have working
alone. Nevertheless, individual work provides the foundation for productive and
synergistic group work. Teams will be formed, with three or four students per team.
These will be used in two ways. First, in-class discussion and reporting on assignments
will be by group (whenever possible). Second, problem set assignments will be group
activities but the submission of assignment outputs will be done individually.
Presentation of output will be done on a rotation basis. All students will evaluate
themselves and their fellow group members with respect to contributions to group
function at least twice during the semester. This evaluation will contribute to the class
standing portion of the course grade and will be used primarily in deciding borderline
grades.
Academic honesty policy
It is a part of your education to learn responsibility and self-discipline, particularly with
regards to academic honesty. The most important issue of academic honesty is cheating.
Cheating is defined to include any attempt to defraud, deceive, or mislead the instructor
in arriving at an honest grade assessment. Plagiarism is a form of cheating that involves
presenting as one's own work the ideas or work of another.
All portions of any test, project, or final exam submitted by you for a grade must be
your own work, unless you are instructed to work collaboratively. Specific requirements
will be described for collaborative projects, but all work presented must be the work of
members of that group. Research materials used must be properly cited. Cheating in a
major course examination by a student will entail a failing mark of F for the given
course. Cheating, dishonesty or plagiarism in papers and other works will entail a zero
(0) score for the said requirement. Policies have been established by Xavier University
to insure due process in charges of cheating or plagiarism. A copy of these procedures
can be found in the Student Handbook.
No-Orientation-No-Lab
Attend the laboratory orientation! At the beginning of the course, there will be
discussion on general lab safety, chemical safety, and the applicable safety regulations.
This is usually conducted by the college through a seminar. Students who failed to
attend the lab orientation must coordinate with the college lab manager to attend the
delayed orientation set by the college otherwise he/she will not be allowed to participate
in any laboratory exercise.
Engineering teams
All activities in this course, except some specific assignments, are to be carried out as a
team effort. Engineering teams will follow these guidelines:
1. Four to five-person engineering teams will be formed at the beginning of the course.
2. All members of the team are expected to contribute to all aspects of the assignment
planning, safety, data collection, analysis, oral presentations, report writing, and
peer evaluation.
3. One member of the team will serve as team leader and coordinate the activities of
the team. He/she will make sure that the methodology is properly implemented and
the objectives for a lab exercise are met. A second team member serving as safety
coordinator will take responsibility for safety issues such as inspecting PPE of their
group members for the safety aspects of the assigned experiment; secure a copy of
MSDS of pertinent chemicals used and conducting the Safety Meeting for that
cycle. These responsibilities will rotate for each experiment. As soon as the teams
are formed, members of the team will select the team leaders and safety
coordinators for the semester and submit the names to the instructor.
4. As each experiment is completed, every team member submits a peer evaluation
form rating the performance of all members of the team and giving comments about
the team activities.
Safety first
Utmost care should be exercised in the laboratory to prevent damage to equipment and
injury to personnel. Each student should be in appropriate Laboratory Attire (gown,
working shirt, gloves, safety gears, etc). A student not in appropriate Laboratory Attire
for a particular activity will be marked absent for the said exercise.
No Hoarse Playing
The apparatuses and equipment used in this course are delicate and expensive. Learn to
handle them properly and treat them with extreme care. Unnecessary activities inside
the laboratory premises are highly discouraged. Otherwise the students will be held
responsible for damage resulting from abuse or misuse.
CLAYGO (Clean-As-You-Go)
Laboratory exercises will be done in teams. It is the responsibility of each team to clean
its own apparatuses / equipment and area where their laboratory work has been
performed.
XU COLLEGE OF ENGINEERING
GENERAL LABORATORY GUIDELINES
I. On Laboratory Protective Clothing/Equipment
It shall be the responsibility of all laboratory workers to always wear appropriate clothing
(e.g. pants, shirts, shoes) and personal protective equipment (e.g. safety glasses,
laboratory coats or aprons, gloves) in the laboratory. Personal protection may vary
according to the activities set forth by the laboratory instructors.
The following should be observed inside the laboratory:
1. The workers personal clothing should be fully covering. Open sandals as well as high
heeled shoes are prohibited, shorts are not recommended.
2. Unrestrained long hair and loose clothing such as neckties and baggy pants are
inappropriate in a laboratory and are therefore prohibited. Such items can catch fire,
be dipped in chemicals and get caught in equipment. Similarly, rings, bracelets,
watches or other jewelry that could be damaged, trap chemicals close to the skin,
come in contact with electrical sources or get caught in machinery should not be worn
in situations where chemicals could be absorbed in the leather and held close to the
skin.
II. On Borrowing Equipment and/or Apparatuses
When performing a regular laboratory exercise, the student, or group of students, should
accomplish the following:
1. Complete Two (2) copies of the Borrowers Form for Equipment and/or
Apparatuses. The borrowers form can be downloaded from the college website.
The Group Leader should fill up the following information:
a. Laboratory/Room This refers to the laboratory where the equipment/or apparatuses
are housed, and/or where the student(s) is/are to performing the exercise.
b. Experiment Title This refers to the name of experiment and/or exercise that is to be
conducted in the laboratory.
c. Subject, Instructor, Schedule, and Date of Actual Use These refer to, respectively,
the subject for which the laboratory exercise is to be conducted, the faculty handling
the subject, the regular laboratory schedule, and the actual date that the laboratory
exercise is to be conducted.
d. Time Checked Out This refers to the specific time that the equipment and/or
apparatuses are checked out. This will facilitate the logistics associated with the
equipment and/or apparatuses.
e. Item Code, Description, Quantity, and Purpose/Remarks Similarly, when
meticulously accomplished, these details facilitate logistics. The Laboratory
Technician fills in the portion for Purpose/Remarks with details as to the general
condition of the apparatuses and/or equipment, or purpose for which the items are
borrowed. Especially noted are slightly scratched or dented apparatuses and/or
equipment so that the group members are not made accountable for said damage.
f. Name and Signature Group members who are actually present, and are to perform
the laboratory exercise, write their names and affix respective signatures on the spaces
provided for.
3. The Group Leader submits the completed form together with his/her University ID
before the instruments and materials are released to the group for the days laboratory
exercise.
4. Upon completion of the activity, the group members return all borrowed equipment
and/or apparatuses to the Laboratory Technician, who then affixes his remarks and/or
signature on both copies of the Borrowers Form, indicating that the borrowed items
are returned in the condition indicated, and hands back the borrowers University ID.
5. The group members must make sure that, upon the return of the equipment and/or
apparatuses, the space indicated for Time Returned is filled out and countersigned by
the Group Leader (the last group recorded to have borrowed an item is accountable
for it, until the return of the same).
6. One copy of the slip is given to the Group Leader, and the other copy retained as file
for the Department by the Laboratory Technician.
III. On Borrowing Equipment and/or Apparatuses for Out-of-Campus Laboratory
Activities
For regular laboratory exercises that require the instrument(s) to be brought outside of the
University campus, the Laboratory Course Instructor submits to the Engineering
Laboratory Manager a request letter, noted by the Department Chair indicating the
description and quantity, and the dates of actual loan and subsequent return, of the
instrument/s.
A. Out of Campus Activity for One (1) Day
The Group Leader submits the completed form together with any ID of the
Laboratory Course Instructor before the instruments are released to the group for the
days laboratory exercise.
B. More than One (1) Day Activity
The completed borrowers form must be accompanied by a Request Letter, noted by
the Laboratory Course Instructor and approved by the Engineering Laboratory
Manager indicating the description and quantity, and the dates of actual loan and
subsequent return, of the instrument/s.
Note: NO EQUIPMENT AND/OR APPARATUS SHALL BE BROUGHT OUT OF
CAMPUS FOR THE CONDUCT OF REGULAR LABORATORY EXERCISES
WITHOUT THE EXPLICIT APPROVAL OF THE ENGINEERING
LABORATORY MANAGER AND THE DEAN.
C. Instruments on loan must be returned on the same day of the scheduled activity, or on
the date stipulated in the approved request letter otherwise the group shall no longer
be allowed to bring any of the Colleges instruments outside the university campus.
The Laboratory Technician affixes his remarks and/or signature on both copies of the
Borrowers Form, indicating that the borrowed items are returned in the condition
indicated, and hands back the borrowers University ID.
D. The group members must make sure that, upon the return of the equipment and/or
apparatuses, the space indicated for Date and Time Returned is filled out and
countersigned by the Group Leader (the last group recorded to have borrowed an item
is accountable for it, until the return of the same).
IV. On Materials, Chemicals and other Consumable Supplies
When the laboratory exercise makes use of materials and other consumable supplies, the
student, or group of students, should accomplish Two (2) copies of the Request Form for
Materials and Supplies should be obtained and filled up by the student or group of
students, at least two weeks before the scheduled date of the exercise. The request form
can be obtained from the Laboratory Technician.
A. All group members sign the Request Form and give it to the Laboratory Course
Instructor for his/her signature and brings it to the Laboratory Technician, who
indicates his Remarks (i.e., hazard or toxicity, special handling requirement, etc.) and
promptly distributes the materials and/or supplies requested for the scheduled
laboratory exercise.
B. Upon issuance of the requested materials and/or supplies, the Laboratory Technician
affixes his signature on the Request Form, gives one (1) copy to the Group Leader,
and retains the other copy as file for the Laboratory Documentation.
C. Laboratory workers shall exercise frugality in utilizing laboratory supplies. All
unused materials that remain unadulterated at the end of the laboratory exercise shall
be returned to the Laboratory Technician.
V. On Request for Extension
An extension may be requested for exercises in progress and whose subsequent
continuation and completion require more than 30 minutes. A laboratory exercise that
extends beyond the allotted period for not more than 30 minutes does not need the
extension request. However since the group members MUST return all borrowed
instruments and/or apparatuses ONLY to the Laboratory Technician (who might
otherwise be engaged elsewhere by then) the group members MUST wait for the
Laboratory Technician to be available for them.
Requests for extension may be granted subject to the following conditions:
1. Availability of Instructors who may supervise the Extended Laboratory Activity
2. Availability of the Laboratory Technicians who will attend to the needs of the
requesting party
For request for extension, the student, or group of students, should accomplish the
following:
1. Two (2) copies of the Request Form for Extension of Use of Laboratory. The
request form can be obtained from the Office of the Engineering Laboratory Manager.
2. It shall be the responsibility of the Laboratory Course Instructor to advise his/her
students on the necessity of accomplishing the Request Form for Extension of Use of
Laboratory. Both the Laboratory Course Instructor and the Department Chair endorse
the request.
3. The students clearly indicate the Date of Actual Use, and obtain the explicit
concurrence of the Laboratory Technician. NO SUCH EXTENSION IS
ALLOWED WITHOUT THE APPROVAL OF THE Engineering Laboratory
Manager.
CONCURRENTLY, NO EXTENSION OF ACTIVITY IS ALLOWED
WITHOUT THE SUPERVISION OF THE LABORATORY ISNTRUCTOR OR
HIS SUBSTITUTE.
4. A student or a group of students with an approved request for extension but who
arrives more than 30 minutes later than the specified time forfeits the entitlement and
shall not be allowed access to the laboratory as scheduled. A request for makeup
shall therefore be filed, following the proper channel.
5. Upon completion of the exercise, the group members return all borrowed equipment
and/or apparatuses to the Laboratory Technician, who the writes his remarks and/or
affixes his signature on both copies of the Borrowers Form, indicating that the
borrowed items are returned in the condition indicated, and hands back the borrowers
University ID.
6. The group members make sure that, upon the return of the equipment and/or
apparatuses, the space indicated for Time Returned is filled out and countersigned by
the Group Leader.
7. One copy of the form and extension request is given to the Group Leader, and the
other copy retained as file for the Department by the Laboratory Technician.
VI. On Breakage, Damage, or Loss of Instrument
1. In cases of breakage, damage, or loss of the instrument and/or apparatuses, the group
members whose signatures appear in the Borrowers Form shall be held liable for the
replacement of the item(s) broken, damaged, or lost.
2. In cases when the whole class concurrently uses an equipment and/or apparatus, the
entire class shall be accountable for the equipment and/or apparatuses.
3. It shall be the responsibility of each group member to ensure that all borrowed
equipment and/or apparatuses are accounted for before they leave the laboratory.
In the same way, the Laboratory Technician shall make sure that all borrowed
equipment and/or apparatuses are accounted for before the students leave the
laboratory.
4. The Laboratory Technician shall submit to the College Administrative Assistant a list
of students with liabilities in the form stated above at least one week before the final
examinations week (i.e., the period allotted for the signing of clearance). The
Department Chair shall be furnished a copy of such list.
NO STUDENT SHALL BE CLEARED BY THE OFFICE OF THE DEAN
UNLESS CLEARED FROM ANY SUCH LIABILITY BY THE COLLEGE
LABORATORY MANAGER.
KEEPING THE WORK AREA CLEAN, SAFE AND IN PROPER ORDER
SHALL BE THE RESPONSIBILITY OF ALL LABORATORY WORKERS.
GUIDELINES FOR SAFETY IN THE

CHEMICAL ENGINEERING LABORATORY
I. PREPARATION
Before starting any laboratory operation ask and answer the following questions by
yourself:
1. Have I done this before?
2. Do I have the proper equipment?
3. Does anything look wrong?
4. What are the hazards?
5. Should I work in a fume hood?
6. Do I need goggles or other safety equipment?
7. Do I need additional help?
8. Should I check further with my instructor?
9. Have I planned this experiment or exercise?
10. Do I know what to do, if there is an accident?
11. Do I know where the fire extinguishers are located?
II. LABORATORY SAFETY RULES
1. NO SMOKING IN THE LABORATORY.
2. Safety glasses will be worn at all times where applicable during laboratory periods.
These glasses will be kept between laboratory sessions in the racks provided.
3. Wear apron (lab overall) in the lab when running apparatus and handling liquids.
4. Wear rubber gloves when handling liquids.
5. When dangerous chemicals are in use, a second person should be within call.
6. Find out the location of First Aid Box.
7. Before operating any valve, switch, etc., know precisely what the effect of your
manipulation will be.
8. Turn off all the valves on cylinders of compressed or liquefied gases when not in use.
9. Students are not allowed to open gas cylinders. Ask the technician.
10. Report all injuries to instructor and to XU doctor immediately. Dial 194.
11. Attach a label "Please leave on" on fittings you need "on" for long time.
12. Keep all inflammable liquids or gases away from open electrical equipment and other
sources of ignition.
13. Gas cylinders must be kept in a stand or chained vertically to a bench.
14. Avoid inhalation of gases or vapors of any kind, especially organic compounds.
15. Do not leave cables trailing across the floor of lab.
16. Practice good housekeeping. Clean all spills at once. Return all equipment to proper
storage when not in use. Place all trash in appropriate receptacles.
17. Avoid direct blasts of air on the skin from high-pressure compressed air lines. Never
play with air hoses.
18. Use special vacuum cleaner from laboratory for immediate removal of mercury spills.
Arrangement should be made to contain mercury.
19. Make sure any system being heated is properly vented
20. Know the location and use of all emergency, protective, and fire fighting equipment.
21. Do not smell directly any chemical being heated.

22. Remember that, if a lab smells, do not use it. Inform the instructor or laboratory
technician immediately.
23. Do not leave the laboratory while an apparatus is on. Always inform the instructor or
the technician if you are in a situation that requires for you to leave the laboratory.
24. Make sure any system being heated is properly vented.
25. Do not wear loose clothing or neckties when working with machinery. You will not
be allowed to enter the lab if you are in loose dress or not wearing covered shoes.
26. Report to the instructor any conditions that are safety hazards.
27. All power wiring is to be installed by an approved electrician.
28. All forms of asbestos should be treated as dangerous.
29. Keep the lab tidy.
30. Always remember: SAFETY IS GOOD TECHNIQUE!
REVISION HISTORY AND ACKNOWLEDGEMENT

Date
Editor
History
June 1, 2015
C.S. Balagtas
Original publishing in
Microsoft Word format
TABLE OF CONTENTS
SECTION TITLE
PAGE
Preface .
ii
General Information About The Laboratory ...
iii
XU College of Engineering
General Laboratory Guidelines
xi
Guidelines for Safety in the Chemical Engineering Laboratory
xvi
Revision History and Acknowledgement ...
xviii
I. CHEMISTRY OF OILS, FATS AND WAX PROCESSING

Expt. No. 1: Coconut Oil Extraction and Refining .....
19
II. CHEMISTRY OF FLAVORS AND FRAGRANCES

Expt. No. 2: Extraction of Essential Oils.
19
III. CHEMISTRY OF SURFACTANTS AND THE MANUFACTURE OF

SOAP AND DETERGENTS
Expt. No. 3: Preparation of Soap....
19
IV. CHEMISTRY OF SACCHARIDES

Expt. No. 4: Refining of Sugar ..
19
V. FERMENTATION PROCESSES AND THEIR APPLICATION

Expt. No. 5: Alcoholic Fermentation .
Expt. No. 6: Preparation of Cheese ...
19
19
VI. PULP AND PAPER

Expt. No. 7: Production of Paper....
19
EXERCISE 1: COCONUT OIL EXTRACTION

AND REFINING
Number of hours required
for completion: ______________
Date started: _________________
Date due: ____________________

Date completed: _____________
INTRODUCTION
An oil is any neutral, nonpolar chemical substance, that is a viscous liquid at
ambient temperatures (eg.room temperature, 20C), and is immiscible with water but
soluble in alcohols or ethers. It is an ester of glycerol, the simplest triol. Its triester is also
known as triglyceride. There are two broad classifications of oils: edible (cooking oil) and
inedible. Oils may be animal, vegetable, or petrochemical in origin, and may
be volatile or non-volatile. One specific source for oil is the coconut.
Coconut oil is produced from extraction of matured coconut meat. Coconut oil
belongs to the group of vegetable oils named lauric oils, which are characterized by a
high level of short-chain fatty acids (>50% C6:0C12:0) and low unsaturation. Because
of its high saturated fat content it is slow to oxidize and, thus, resistant to rancidification,
lasting up to two years without spoiling. Traditionally, coconut oil is produced through
fermentation. In this experiment, students are to produce coconut oil using wet milling
method followed by filtration using activated charcoal.
MATERIALS AND APPARATUSES
1 kg grated coconut
Filter paper
meat
Activated charcoal
Beaker
Funnel
Stove
Cooking pot
Stirring spoon
Strainer
Glass
bottle/container
PROCEDURE
Extraction of the coconut oil
1. Wrap the raw coconut meat in cheesecloth prior to extraction.
2. Using a filter press squeeze out the coconut milk into a metal pan.
3. Place the coconut milk in a double boiler (water bath) and heat very slowly to
coagulate the protein and release the oil. After this, the coconut protein (latik) will
coagulate and the oil will separate out. For the first hour of heating, temperature can be
allowed to reach 90oC. After this time the temperature should not exceed 80oC until the
protein begins to coagulate. Heating should be done in such a way that the contents of the
pan will just simmer and not boil.
4. Lower the temperature to 60oC when the oil starts to separate from the coagulated
protein. Do not allow the latik to turn brown.
5. Separate the oil from the solids by straining the mixture through a muslin cloth or in a
stainless steel screen with fine mesh over a stainless steel pot. Set aside the solids.
Refining process
6. The filtered oil will be subjected to another filtration using a filter paper layered with
an adequate amount of activated charcoal. The dosing of the carbon should lie between
0.5 and 1.5 percent by mass.
7. The oil will be left to trickle down the funnel into a beaker. This should be clear-water
coloured oil.
8. Finally, weigh the oil in the top loading balance and calculate the %yield.
Note: Keep a record of the weights of each material used during the experiment.
GUIDE QUESTIONS FOR DISCUSSION
1. What is/are the constituents of a coconut milk?
2. What is/are the main constituent of the coconut oil produced?
3. What is/are the constituents of the latik? Why did it coagulate after heating? Explain.
4. What will happen if the temperature during heating is not maintained?
5. Using material balance, how much oil should have been produced theoretically?
6. What is the actual yield?
7. What made the actual yield higher/lower than the theoretical?
8. What should have been done to improve the experiment? (if there is any)
References:
http://www.thepurificationcompany.com/files/know%20how/2002-2b%20norit%20responds%20to%20signals%20from%20the%20market.pdf [Retrieved: 25 August 2015]
http://www.fao.org/docrep/v4700e/v4700e0a.htm [Retrieved: 8 July 2014]
http://lib3.dss.go.th/fulltext/Journal/J.AOCS/J.AOCS/2000/no.6/jun2000vol77,no6,p581-586.pdf [Retrieved: 8 July 2014]
ftp://ftp.fao.org/docrep/fao/009/ag094e/ag094e00.pdf [Retrieved: 8 July 2014]
EXERCISE 2: EXTRACTION OF ESSENTIAL OILS

Date started: _________________
Date due: ____________________

INTRODUCTION
An essential oil is the essence of a plant which produces its characteristic aroma.
Essential oils have been extracted from plants and spices such as allspice, almond, anise,
basil, bay, caraway, cinnamon, cumin, dill, eucalyptus, garlic, jasmine, juniper, orange
(and other citrus), peppermint, rose, rosemary, sassafras, sandalwood, spearmint, thyme,
violet, wintergreen, and more, and valued since ancient times. Extraction processes can be
done by simple solvent extraction by soaking spices or flowers in water, alcohol, or oil
and distillation.
In this experiment, we will be extracting essential oils through the process of
expression and hot maceration. Essential oils are then either added to alcohol or an oil
base when making perfumes. The percentage of essential oil used in perfumes is high, and
to prevent any allergic reaction, remember to do a skin patch test.
MATERIALS AND APPARATUSES
For Expression:
For Perfume/Cologne
Citrus fruits peelings
Preparation:
Vial/Container with cap
Blue or amber glass
or cork
bottles
Jojoba oil [or a
Cork stopper
vegetable oil]
11 ml alcohol/vodka
Separatory funnel
(or jojoba oil for an
oil-based perfume)
For Hot Maceration:
Aromatic plant materials
Vegetable or animal fat
PROCEDURE
Solid-Liquid Extraction (or Leaching)
1. Place 3 or 4 boiling chips into the round bottom flask. Fill this
with distilled water at approximately 75% of its volume.
2. Chop the sample into smaller size. Weigh out the sample
before placing it into the thimble.
3. Close the extraction thimble with a fat-free cotton wad.
4. Insert the thimble into the Soxhlet extractor. If the Soxhlet
extractor has a spigot for solvent draining, close the spigot.
5. Assemble the Soxhlet extraction setup (see Figure 1).
6. Extract for several cycles at a temperature of 110-1300C for
approximately 1.5hours or until all of the water has been
Figure 2.1. Soxhlet
Extraction Setup
(Image taken from 3

http://www.behrlabor.com/pdf/app_extrakti
on_gb.pdf)
evaporated and condensed in the Soxhlet extractor. At this point, most of the oil was
collected in the round bottom flask.
7. Collect the oil-water mixture into a suitable vessel.
8. Place the vessel in a drying oven at 10320C and heat to constant weight. Do not
forget to cool the vessel to room temperature before weighing. Observe carefully all
safety guidelines concerning the use of the oven.
9. Calculate the %yield.
Expression
1. Press the peels to obtain the oil emulsion directly into a separatory funnel. Pour oil.
2. Extract the essential oil with jojoba oil by adding 10 mL of jojoba oil to the separatory
funnel. Stopper and shake well, venting every few shakes.
3. Allow the layer to separate. The jojoba oil layer will be on top.
4. Drain the water layer into a container. Drain the jojoba oil layer into a vial/container.
If the jojoba oil extract is cloudy, dry the extract with a small amount of anhydrous
sodium sulfate.
5. Cap or cover the vial or container.
6. Label the container. This mixture is an essential oil extract and will be used in the
preparation of a perfume/cologne/flavor.
Hot Maceration
Certain plant materials require maceration in warm water before they release the essential
oils, as their volatile components are glycosidically bound. For example, leaves of
wintergreen (Gaultheria procumbens) contain the precursor gaultherin and the enzyme
primeverosidase; when the leaves are macerated in warm water, the enzyme acts on the
gaultherin and liberates free methyl salicylate and primeverose. Other similar examples
include brown mustard (sinigrin), bitter almonds (amygdalin) and garlic (alliin).
1. Immerse aromatic plant materials in molten fat heated at 45-60 C for 1 to 2 h.
2. After each immersion, filter the fat and separate from the plant materials.
3. After 10 to 20 immersions, separate the fat from waste plant material and water.
For a perfume you will use around 15% essential oil, whilst for a lighter eau de toilette
you will use about 4 - 8% essential oil and a yet lighter eau de cologne 1 - 5%.
Materials:
Perfume/Cologne Preparation
1. Place the alcohol/vodka base into a glass mixing container.
2. Add the essential oils and mix well.
3. Bottle, cap and leave the mixture for 4 days, giving the bottle a gentle shake every
day.
1. What are the different essential oil extraction processes? What are their advantages
and disadvantages?
2. Why do extraction processes vary with the kind of raw material?
4
3. What is the main constituent of the oil that you have obtained?
4. What was your estimated %yield? How efficient is the extraction process?
References:
http://cst.ur.ac.rw/library/Food%20Science%20books/batch1/Food%20Analysis%20Laboratory%20Manual
%20Second%20Edition.pdf [Retrieved: 25 August 2015]
http://www.behr-labor.com/pdf/app_extraktion_gb.pdf [Retrieved: 25 August 2015]
http://www.essentialoils.co.za/recipes.htm [Retrieved: 15 July 2014]
http://www.essentialoils.co.za/enfleurage.htm [Retrieved: 15 July 2014]
http://www.chymist.com/Laboratory%20Experiments.htm [Retrieved: 15 July 2014]
http://www.chymist.com/Isolation%20of%20an%20Essential%20Oil.pdf [Retrieved: 15 July 2014]
http://agritech.tnau.ac.in/horticulture/extraction_methods_natural_essential_oil.pdf [Retrieved: 15 July
2014]
http://www.ebay.com/gds/Common-Perfume-Ingredients-Decoded-/10000000177632555/g.html
[Retrieved: 16 July 2014]
http://en.wikipedia.org/wiki/Perfume [Retrieved: 16 July 2014]
EXERCISE 3: PREPARATION OF SOAP

Date started: _________________
Date due: ____________________

INTRODUCTION
Soap is a salt (or a mixture of salts) of fatty acids. These fatty acids, of which
there are about 20 naturally occurring members, are carboxylic acids containing 14, 16, or
18 carbon atoms in an unbranched chain. The even numbered chains result from the
polymerization of a 2-carbon acetate unit during fat synthesis in cells.
Soap is prepared by hydrolyzing a fat under alkaline conditions through a reaction
called saponification. The fats and oils most commonly used in soap preparation are lard
and tallow from animal sources, and coconut, palm and olive oils from vegetable sources.
The length of the hydrocarbon chain and the number of double bonds in the carboxylic
acid portion of the fat or oil determine the properties of the resulting soap. For example,
a salt of a saturated, long-chain acid makes a harder, more insoluble soap. Chain length
also affects solubility. Tallow is the principal fatty material used in soap making, with
coconut or palm oil blended in, to produce a softer (more soluble) soap which will readily
lather. Soaps made with KOH (caustic potash) instead of NaOH (caustic soda) are liquid
rather than solid, at room temperature.
This experiment is an introduction to the industrial method of making opaque and
transparent soap using the cold and hot processes, the two most commonly used
methods to make soap. Both require a heat source and careful calculations to ensure that
no caustic base is left unreacted in the soap. The hot process uses heat to speed the
reaction resulting in fully saponified soap by the time the soap is poured into molds. The
cold process uses just enough heat to ensure that all the fat is melted prior to reacting it
with the base.
MATERIALS AND APPARATUS
Fats and Oils (Castor, olive, palm
and coconut oils if possible)
NaOH
1%w/w CaCl2 and MgCl2 solutions
Scent
Distilled (if not deionized) water
Mold or weighing boats
Thermometer
pH meter
Hot plate
Stirring rod/stirrer/spatula
Optional: Oats and food coloring
Graduated cylinder (or measuring

cup)
Crockpot
Beaker and tongs
Test tubes
Watch glass
Petroleum
jelly/parchment
paper/cling wrap
Filter paper/Cheesecloth
Iron stand and clamps
Erlenmeyer flask
SAFETY PRECAUTIONS
1. Wear your personal protective equipment throughout the experiment since NaOH can
cause permanent eye damage. Sodium hydroxide is caustic and can cause serious
burns. On contact, flush affected area with water.
2. Watch your reaction mixture at all times. Do not let it boil over and do not let the
volume of the heated solution decrease too much during saponification. Using a
marker, draw a line on the outside of the flask or pot to indicate the level of liquid. If
the level drops, add more ethanol slowly to bring the level to the line.
3. When using a thermometer in this experiment, never use it to stir liquids. Instead, use
a fire polished glass rod. To properly measure the temperature of a liquid, hold the
thermometer so that its bulb is suspended in the center of the liquid while reading the
mercury level. If the liquid is being heated on a hot plate, do not let the thermometer
bulb to rest on the bottom of the container, as it will then be overheated. Remove the
thermometer from the container after each reading.
4. Ethanol and essential and fragrance oils are flammable. Keep away from sources of
fire.
5. Waste ethanol and sodium hydroxide solution (if any) should be disposed of in the
organic waste containers.
PROCEDURE
I. Saponification
I.A. Cold Process
1. Decide which oil/oils you will be using. Each oil has differing properties that react
differently and produce different qualities in your soap. For example, coconut oil will
give you a hard bubbly bar with excellent cleaning properties; however, bars with
more than 40% coconut oil can be drying to the skin. On the other hand, olive oil
makes a super moisturizing soap but the bar is softer, doesnt last as long, and can
leave behind an oily feeling. 100% olive oil bars also take considerably longer to
react. In general, oils that are great for cleaning produce a harder bar but arent that
moisturizing, while moisturizing oils produce softer bars and dont clean as well. 30%
coconut oil and 70% other oil/oil blend reacts easily and makes a great all around bar.
2. Before starting, calculate the amount of base and water required to make soap out
of 50.0g of oil material, either 100% or a mixture of different oils. Use a 5% excess of
the oil (superfatting) to ensure that nearly all of the sodium hydroxide is consumed
in the saponification process. Otherwise, the soap will be too basic and could be
harmful to use. The excess oil is also great for the skin. For most soaps, a good
amount of water is 35% of the mass of oil used.
To calculate the amount of NaOH required, you must refer to Table 1 below. The
figures in the third column (NaOH Bar Soap) give the grams of base required to
saponify 1 gram of the oil. For example, 1.0 gram of beef tallow would require 0.140
g of solid NaOH. If 100 g of beef tallow were used, then the amount of NaOH
required (assuming a 5% excess of oil) would be 95 g oil x 0.140 g NaOH/1.0 g oil =
13.3 g of solid NaOH.
It is sometimes desirable to use more than one kind of oil. Here are the calculations
for a soap containing 30% coconut oil and 70% olive oil. Assume that 70 g of coconut
7
oil and 30 g of olive oil are used. First, calculate the mass of 95% of each oil to ensure
that there is a 5% excess of oil. Then do the following calculation: 28.5 g coconut oil
x 0.181 g NaOH/g oil + 66.5 g olive oil x 0.134 g NaOH/g oil = 5.16 g + 8.91 g =
14.07 g NaOH required. The recipe would be 30 g of coconut oil, 70 g of olive oil,
14.06 g NaOH, and 35 mL of water.
Table 1. Saponification numbers of Some Oils
NaOH
KOH
Oil
SAP
(Bar Soap)
(Liquid Soap)
Beef Tallow
190 - 200
0.140
0.196
Canola Oil
0.132
0.187
Castor Oil
175 - 187
0.127
0.179
Coconut Oil
250 - 264
0.181
0.256
Corn Oil
0.135
0.190
Jojoba, Organic
91 - 93
0.068
0.096
Lard
0.141
0.199
Olive Oil A
184 - 196
0.134
0.190
Palm Oil
190 - 205
0.144
0.203
Peanut Oil
0.136
0.190
Soybean Oil
190
0.134
0.188
3. Prepare your mold, anything that will hold its shape will do. You will want to
either grease your mold with petroleum jelly or parchment paper, or plastic wrap. DO
NOT use aluminum foil because it will react with your base and release hydrogen gas.
4. Make your aqueous base solution. Weigh out the amount of NaOH calculated and
put aside. Then pour distilled water into a 250-mL beaker. Slowly add the base to the
water (never water to base!) while swirling or stirring with a glass stirring rod until
dissolved and let cool to 33-43C.
Caution: NaOH is caustic and can burn you! It is harmful to the eyes. Wear
gloves and eye glasses! When NaOH is dissolved in water, a lot of heat is given
off. This solution may become very hot.
5. Weigh and place oils into a beaker and melt/heat on a hot plate to 33-43C.
Mixing the oils and base at similar temperatures facilitates the reaction and prevents
separation.
6. Once both the base solution and your oils are 33-43C, you can begin slowly
pouring the aqueous base solution into the oils while stirring. Continue stirring until
the mixture begins to thicken and you can see trails of your mixture on the surface
upon lifting your spoon/stirrer above the surface. This stage is called trace and some
oils take longer than others to reach this stage. To test for trace, dip a stirring rod into
the mixture and wave it over the surface. If the drizzled material leaves a pattern on
the surface before sinking, the soap has traced.
7. Once you have reached trace, add any of the fragrances or additives, mix
thoroughly, then pour into your mold. Optionally you can chill the mixture at this
point to prevent the soap from going through a gel stage which occurs when the
reaction heats up, turning the soap transparent for a short time before turning opaque
again.
8
Though safe to use at this point, curing for weeks will react any trace amounts of base
and evaporate excess water, resulting in a smoother and longer lasting bar. During
this time a powdery layer of NaCO3 (soda ash) will form on the surface, as residual
NaOH reacts with CO2 in the air while the soap is drying. This powdery layer should
be sliced off and the soap is ready to be used.
8. Weigh the soap and determine the yield.
I.B. Hot Process
1. Half fill a pot with water and place on the hot plate. When the water begins to
boil, adjust the heat, so that the water boils gently, but continuously. While waiting
for the water to boil, weigh a 250ml Erlenmeyer flask on a triple beam balance and
add coconut oil (4.50g), palm oil (6.00g), olive oil (1.50g) and castor oil (3.00g) to it.
2. In a beaker prepare 30 ml of a 50-50%v/v solution of alcohol-water. Cover lid
with watch glass.
3. Weigh and add 2.27g of NaOH pellets to a flask with 5g of distilled water.
Handle NaOH with care as this can burn the skin and is especially harmful to the
eyes.
4. In the hood, mix the NaOH solution to 10 ml of the of the 50-50 alcohol-water
solution to it. Stir the mixture until a transparent solution is formed. Caution: the
beaker will get very hot as the lye dissolves.
5. Pour the lye solution into the Erlenmeyer flask containing the fat and mix well
using a stirring rod or by swirling with a beaker tongs.
6. Clamp the flask in the boiling-water bath and with occasional stirring; allow it to
cook for at least 30 minutes. While the mixture boils, some foam will form (due to
soap formation). Try to minimize excessive foaming, by adding small portions of
alcohol-water solution. The reaction is complete when oil globules are no longer
visible mixture is stirred.
7. Half fill a 600 ml beaker with 300 ml of clear (filtered) saturated salt (NaCl)
solution and 50 ml of water. Pour the still hot reaction mixture containing soap,
glycerine, excess NaOH, and alcohol into the salt solution. Stir the resulting mixture
and allow to stand for 5-10 minutes. The soap will collect as a white layer on the
surface of the salt water in the beaker.
8. Filter the soap preparation either manually or by using a suction trap from the
vacuum flask. Wash the crystals on the filter with 5 ml portions of ice-cold water.
Press out any remaining moisture from the cake of filtered crystals. Allow the product
to air dry for 10-15 minutes.
9. With the help of a clean spatula, transfer the soap crystals to a large sheet of
smooth paper. Pick up the sheet and slide the crystals into a clean, dry 150 ml beaker.
Let the beaker stand, uncovered for several days to air-dry the product.
I.C. Preparation of Transparent Soap
1. Weigh 3.71g of glycerine and 6.04g alcohol in the fume hood.
2. If the pH is ok, dissolve the hot-processed soap by slowly pouring the glycerin
and alcohol to the soap-making pot. Mix everything thoroughly until all the soap is
9
dissolved in the solvent. Caution:alcohol is highly flammable. Wear personal

protective equipment. Make sure work area is properly ventilated.
3. Let the mixture set on low heat for 30minutes. Cover the pot with lid.
4. While waiting, prepare the sugar solution. Dissolve 5.56g sugar in 4.82g distilled
water in a pot or container.
5. Add half of the sugar solution to the soap solution and mix well.
6. Skim off the sticky foam from the top of the mixture--this can be used as soap
after cooling.
7. Test for transparency: Take a cold/frozen glass and pour about one tablespoon of
soap on the bottom. If milkiness is evident, add more sugar solution in small amounts
and repeat the test. If milkiness is more pronounced, switch to glycerine and alcohol.
Do not add too much solvent because this causes sweating.
8. When the transparency is ok, the coloring and scent may be added.
10. Finally, pour the soap into molds. When the soap is cooled and solid, unmold it
and let it age for a week. The water and alcohol will eventually evaporate and the
soap will become harder.
II. SOAP QUALITY TESTS
II.A. Preparation of Soap Solutions
In this part of the experiment, you will be comparing the properties of the soap you
made with a commercial soap and a detergent. You will start out by making three
separate soap solutions, as detailed in the following steps:
1. Mix 1 g of the soap you prepared with 50 mL of warm deionized water. Swirl the
solution to mix it well (but try not to shake it, because you dont want to make lots of
suds yet). Label this solution.
2. Mix 20 drops of the pink liquid lab soap with 50 mL of warm deionized water.
Swirl this solution to mix it well. Label the flask.
3. Mix 1 g of the commercial detergent with 50 mL of warm deionized water, and
swirl to mix well.
II.B. pH Test
1. Before using your soap, you must test the pH to make sure that it is not too basic.
Soaps with a pH > 10 can be irritating to the skin depending on skin type. Soaps
with a pH > 11 should NOT be used on the skin. They can be grated and used as
laundry soap which generally has a pH of 10-12.
2. Label four separate test tubes.
3. In the first tube, place 10 mL of the soap solution you made. In the second tube,
place 10 mL of the commercial soap solution. In the third tube, place 10 mL of the
detergent solution. In the fourth tube, place 1mL of deionized water (this will be the
control).
4. Swirl each solution and then read the pH using pH meter. Record the pH of each
solution. Save these solutions for the next part.
II.C. Foam Test
10
1. Stopper each of the tubes from pH test and shake each one continuously for
10seconds.
2. Observe and record the amount of suds or foam each soap solution produces. Save
these solutions for the next part.
II.D. Interaction with Oil
1. Add 5 drops of oil to each test tube from foam test.
2. Stopper and shake each of the tubes continuously for 10 seconds.
3. Observe what happens to the oil layer in each tube. Compare the amount of suds
in each tube to the amount of suds they each had in the foam test. Do the tubes have
more or less suds than they did before? Which substance(s) dispersed (emulsified) the
oil? These solutions can be poured down the sink.
II.E. Hard Water Test
1. Label three clean test tubes. Put 5 mL of your soap solution in the first, 5 mL of
commercial soap solution in the second tube, and 5 mL of detergent solution in the
third.
2. Add 20 drops of 1% CaCl2 solution to each tube. Stopper each test tube and shake
continuously for 10 seconds.
3. Compare the amount of suds in each tube to the amount of suds they each had in
previous tests. These solutions can also be poured down the sink. Wash and rinse the
test tubes.
4. Repeat step 2 with new samples of each soap solution, but instead of adding 1%
CaCl2 solution, add 20 drops of 1 % MgCl2 solution. Record your other observations
as before. Pour these solutions down the sink and wash and rinse the test tubes.
1. What is/are the main constituent of the oil/s you used?
2. Write the reaction for the saponification of your oil/s with sodium hydroxide. Why is
the product of saponification called a salt?
3. Why was ethanol added to the reaction mixture of fat and base?
4. What is/are the main constituents of the soap you produced?
5. What is your %yield? What made it higher or lower than the theoretical?
6. Why is distilled/deionized water used in the preparation of the soaps? What effect
would ordinary tap water have on the preparation of the soaps?
7. Using the same weights of fat and alkali, would you get more or less soap by using
KOH instead of NaOH?
8. Do you think the solid soap that you made contains glycerol? Why or why not?
Explain.
9. Did the solid soap you made contain excess base? Explain how you know.
10. Explain what happened in the quality tests. Did any of the soap solutions work better
than the others?
References
Suzanne T. Mabrouk, Journal of Chem. Ed. 2005, 82 (1534-1537)
11
Ghaim, J. B.; Volz, E. D. Skin Cleansing Bars. In Handbook of Cosmetic Science and Technology; Barel,
A. O., Paye, M., Maibach, H. I., Eds.; Marcel Dekker: New York, 2001; p 493.
Piso, Z.; Winder, C. A. Soap, Syndet and Soap/Syndet Bar Formulations. In Soap Technology For The
1990s; Spitz, L., Ed.; American Oil Chemists Society: Champaign, IL, 1990; p 217.
Cavitch, S. M.The Chemistry of Soapmaking. In The Soapmakers Companion; Storey: Pownal, VT, 1997;
p 238.
Davidsohn, J.; Better, E. J.; Davidsohn, A. The Fatty Raw Materials: Introduction. In Soap Manufacture;
Interscience Publishers: New York, 1953; Vol. I, pp 206211.
Use of Natural Fats and Oils in Cosmetics. In Baileys Industrial Oil and Fat Products, 5th ed.; Hui, Y. H.,
Ed.; Wiley & Sons: New York, 1996; Vol. 5, pp 366367.
Altman, P. L.; Dittmer, D. S. Fats and Oils: Properties and Composition. In Biology Data Book, 2nd ed.;
Federation of American Societies for Experimental Biology: Bethesda, MD, 1972; Vol. I, pp 348353.
From Nature With Love, Mango Butter. http://www.fromnaturewithlove.com/soap/product
.asp?product_id=butmango(accessed Jun 2005).
Gupta, S. Soap, Chemistry, Chemical and Physical Properties & Raw Materials. In Soap Technology For
The 1990s; Spitz, L., Ed.; American Oil Chemists Society: Champaign, IL, 1990; pp 5758.
p 246.
p 247.
Milwidsky, S. Analytical Tests on Soapmaking Raw Materials. In Soap and Detergent Technology; HAPPI:
Ramsey, NJ, 1980; p 16.
Makela, C. Preparing To Put Milk into Soap. In Milk-Based Soaps: Making Natural, Skin-Nourishing Soap;
Storey: Pownal, VT, 1997; pp 3132.
Cavitch, S. M. Making Transparent Soaps. In The Soapmakers Companion; Storey: Pownal, VT, 1997; p
79.
Failor, C. All About Soap. In Making Transparent Soap: The Art of Crafting, Molding, Scenting, &
Coloring; Storey: Pownal, VT, 2000; p 7.
http://curious-soapmaker.com/how-to-make-transparent-soap.html [Retrieved: 28 July 2014]
http://www.google.com.ph/url?sa=t&rct=j&q=&esrc=s&source=web&cd=12&cad=rja&uact=8&ved=0CC
AQFjABOAo&url=http%3A%2F%2Fcheminnerweb.ukzn.ac.za%2FLibraries%2FCHEM210_Module_des
criptor%2FPrac_manual_v1.sflb.ashx&ei=XgnWU6rGKNjq8AWt5oLoCg&usg=AFQjCNGPxw7lVAjY65
dKAjrTqXmEqzrU0w&bvm=bv.71778758,d.dGc [Retrieved: 28 July 2014]
http://www.google.com.ph/url?sa=t&rct=j&q=&esrc=s&source=web&cd=18&cad=rja&uact=8&ved=0CE
UQFjAHOAo&url=http%3A%2F%2Fwww.baruch.cuny.edu%2Fwsas%2Facademics%2Fnatural_science
%2Fchm_1000%2F9_soap.doc&ei=XgnWU6rGKNjq8AWt5oLoCg&usg=AFQjCNHGtrCtQ9XRcb8Lw8
mh9jCcv_xyxw&bvm=bv.71778758,d.dGc [Retrieved: 28 July 2014]
http://www.mycrandall.ca/faculty/MSchriver/lectures/JCEd2005Soap.pdf [Retrieved: 28 July 2014]
http://www.laney.edu/wp/cheli-fossum/files/2012/01/13-Saponification.pdf [Retrieved: 28 July 2014]
http://facweb.northseattle.edu/jpatterson/pdf/chem252p/252Preparation%20of%20%20Soap10.pdf
[Retrieved: 28 July 2014]
http://en.wikipedia.org/wiki/Pears_soap [Retrieved: 28 July 2014]
12
EXERCISE 4: REFINING OF SUGAR

Date started: _________________
Date due: ____________________

INTRODUCTION
The word "sugar" used in everyday life refers to the chemical sucrose. Sucrose is a
member of a group of substances generally known as polysaccharides, which contain up
to ten monosaccharide units. Monosaccharides are carbohydrates that cannot be further
hydrolysed. All sugars are crystalline, water soluble and sweet tasting.
Sugar was first manufactured from sugar cane in India around 510 B.C, and its
manufacture has spread from there throughout the world. In sugar refining, all impurities
and surrounding plant matter are removed leaving only sucrose. Glucose and fructose are
regarded as impurities due to the difficulty in crystallising them from solution. Sucrose
can be hydrolysed in acidic solution (i.e. below pH 7) to form the glucose and fructose
that is why strict process control, particularly of pH, is maintained in processing.
In this experiment, students will learn the basic processes involved in the refining
of sugar such as affination, clarification, decolorization, evaporation, and crystallization.
Sugar cane stalks
Granulated sugar (for affination and
crystallization)
Phosphoric acid
Calcium hydroxide
Activated carbon
Distilled water
Knife
Chopping board
Rollers or filter press
Cheesecloth
Cooking pan or kettle
Hot plate
Stirrer/spatula
Filter paper
Funnel
Graduated cylinder
pH meter
Thermometer
METHODOLOGY
1. Wash the cane to remove mud and debris. Let it dry and weigh out the amount of raw
material used.
2. Chop the sugarcane stalks into chunks. Next stripped off the hard green outer coating
to reveal the canes porous white center. Again, weigh out the amount of material
produced.
3. Extract the sugar cane juice by putting the chunks in cheesecloth and then repeatedly
pressing using rollers or filter press. Warm water may be added to help macerate the
sugar cane chunks and aid in the extraction or leaching. This process is similar to the
extraction of oil from grated coconut meat.
13
4. The resulting fibrous mass or bagasse must be set aside for weighing. This may be
burned as fuel or as raw material for making paper later on. Always take note of the
amount of materials added and consequently produced along the processes.
5. The next step is affination, derived from a French word meaning refining. Mix
saturated syrup of 60 to 800Brix to the solution to soften the adhering film of
molasses. This dissolves little or none of the sugar but softens or dissolves the coating
of impurities. Remove the resulting syrup by either filtration or centrifugation.
6. Dissolve (or melt as used in refineries) the sugar cake in about half of its weight
with hot water.
7. Clarify this solution by adding calcium hydroxide. The pH must be maintained
between 7-9. Below pH 7 sucrose is hydrolysed to the reducing sugars glucose and
fructose, whereby crystallization of solid sugar tends to become difficult. While above
pH 9, alkali destruction of sugars occurs and coloured components are formed
because of Maillard reaction. Then add enough phosphoric acid to precipitate out the
calcium phosphate. The reaction is 2H3PO4 + 3Ca(OH)2 --> Ca3(PO4)2(s) + 6H2O(l).
The calcium phosphate particles entrap some impurities and absorb others, and then
float to the top of the solution, where they can be skimmed off and consequently
thicken the syrup. Take note of the pH of the solution.
8. Pour the resulting solution on a cooking pan and start the heating process at 650C.
9. During the first minutes of cooking, dregs (residue from the pulverized cane stalk)
will begin to rise and allowed to form as thick dreggy foam (scum) on top of the juice.
Start skimming this foam. Closely regulate the heat in order to maintain the
accumulation of thick foam on top of the juice without bringing the juice to a boil.
After approximately 30 minutes, remove the mixture from heat and cool down in
water bath. The solution is now ready to undergo decolorization.
10. Filter the clarified juice through either granular activated carbon (GAC) or powdered
activated carbon (PAC). Some remaining color-forming impurities adsorb to the
carbon. The purified syrup will now be repeatedly concentrated to supersaturation
before crystallization.
11. Pour 1/3 of the clarified and decoloured juice on a cooking pan or kettle and start the
heating process to about 98-1300C. When the juice has been cooked down (after apx.
1 hour), removes the pan or the kettle from the hot plate and refills it with juice and
then cooked down again. After performing two to three refills, you will be finally
cooking down to heavy syrup. Take note of the appearance of the mixture.Closely
regulate the heat in order to prevent burning the syrup causing heat coagulation which
appears as a dark brown settlement in the syrup.
12. As the juice nears syrup, it will darken and begin to "fall" below the kettle rim. Check
the thickness to determine the proper time to perform the "strike" (remove from
heating and take up the syrup). At this point, the thickness of massecuite would be
similar to a mixture of sugar with 10% water at 98-1300C.
13. After performing the strike, transfer the massecuite into another container in cold
water bath where it would cool and crystallize. Stir frequently until the syrup has
significantly cooled. Small quantity of sucrose granules can be added to the syrup
while hot (commonly called shock-seeding) to help initiate/facilitate the
14
crystallization process. After the syrup has crystallized, chip out the sugar and placed
it in cheesecloth for further draining/refining. The by-product is molasses.
1. What is/are the main constituent of the raw material you used?
2. What happens during affination?
3. What happens during clarification?
4. What happens during evaporation?
5. What happens during crystallization?
6. How much granulated sugar have you produced?
7. What is your actual yield? What made it lower or higher than the theoretical yield?
References
http://nzic.org.nz/ChemProcesses/food/6E.pdf [Date accessed: 19 August 2014]
http://zesterdaily.com/health/the-great-sugarcane-experiment/ [Date accessed: 19 August 2014]
http://www.fssai.gov.in/Portals/0/Pdf/15Manuals/BEVERAGES,%20SUGARS%20&%20CONFECTINER
Y.pdf [Date accessed: 19 August 2014]
http://www.globalhealingcenter.com/sugar-problem/refined-sugar-the-sweetest-poison-of-all
[Date
accessed: 19 August 2014]
http://www.ehow.com/how_2267326_make-sugar-from-sugar-cane.html [Date accessed: 19 August 2014]
http://en.wikipedia.org/wiki/Sugarcane [Date accessed: 19 August 2014]
http://www.southernmatters.com/sugarcane/bulletins/Pope/cane_syrup.pdf [Date accessed: 19 August 2014]
https://www.westernsugar.com/pdf/Refining%20and%20Processing%20Sugar.pdf [Date accessed: 19
August 2014]
http://en.wikipedia.org/wiki/Sodium_bicarbonate [Date accessed: 19 August 2014]
15
EXERCISE 5: ALCOHOLIC FERMENTATION

Date started: _________________
Date due: ____________________

INTRODUCTION
Fermentation in wine-making is the conversion of sugar, by the interaction of
yeasts, into alcohol with a by-product of carbon dioxide (CO2) gas. The chemical reaction
is C6H12O6 2C2H5OH + 2CO2.The usual raw material for alcohol production, aside
from sugar-producing plants (saccharine material) such as sugar beets, sugarcane, fruits,
are cereal grains such as corn, wheat, rye, barley, milo (sorghum grains), rice, potatoes of
all kinds, artichokes, and other high-starch vegetables. A third source of fermentable
sugars is cellulose, as found in wood and waste sulphite liquor. This more complex
process requires the use of acids to reduce the material to wood sugars.
Primary fermentation lasts for approximately one week; during that time most of
the sugars originally present in the mash/must is converted to ethanol and yeast cells, with
the evolution of carbon dioxide. The excess yeast cells are then removed from the juice
along with other sediment, and a slower secondary fermentation is allowed to proceed to
develop the final flavor. Sugar may be added to the original must to achieve the desired
alcohol content or to modify the flavor. The type of wine can be classified according to
the color of the wine. Another classification is based on the starting sugar content, as
listed in Table 1.
Table 1. Classification of wines according to the sugar
Fermentation
is
content.
completed when all the
Specific
Sugar Content
fermentable sugars have been Type
Gravity
(wt%)
converted to alcohol. This end
Dry Wine
1.085 - 1.100
21 - 25
point is measured chemically
Medium Sweet Wine 1.120 - 1.140
29 - 33
by gas chromatograph or
Sweet Wine
1.140 - 1.160
33 - 37
similar methods. Once the
wine is deemed free of fermentable sugar, i.e. dry it is cooled to 4 oC and the dead yeast
cells (known as gross lees) are allowed to settle. The relatively clear wine is then racked
to remove the gross lees before it is stabilized and filtered ready for bottling. In this
experiment, students will prepare an alcoholic beverage out of their chosen raw material.
Equipment
Measuring cup
Sterilized bottles
Cheesecloth or kitchen sieves
Rubber stoppers and tubing
Hydrometer
Balance
Test tube
Reagents
Starchy or glucose-rich raw material
(i.e. fruit juice, starch feedstock, etc.)
Sucrose
Active dry yeast (Saccharomyces
cerevisiae)
Distilled water
Lime water
16
PROCEDURE
1. Prepare Starter Yeast Culture. Dry wine yeast may be directly added to mash from a
package at the level of 1 g per 4 liter of mash. For best results, first suspend 1 g of dry
wine yeast in 10 ml of warm water at about
35 C. Then add the suspended culture to Table 2. Proofs of Alcoholic
mash. Let the yeast grow in a loosely capped Beverages
Proof
sterilized bottle or container at room Beverage
Beers (3-10%v/v)
6-20
temperature.
16-28
2. Prepare an aqueous solution of the raw Wines (8-14%v/v)
32-44
material necessary for the preparation of the Fortified Wines (16
desired alcoholic beverage. Table sugar may 22%v/v)
be added to increase the sugar content of the Spirits (20-70%v/v)
40-140
mash. You may refer to the reaction Fruit Juice < 0.1%v/v
<0.2
presented above and Table 2 for this. For
raw materials such as grains, this must be ground before mashing to expose the starch
granules and help them remain in suspension in a water solution. Potatoes and similar
high-moisture starch crops should be sliced or finely chopped. Since potato starch
granules are large and easily ruptured, it isn't necessary to maintain the hard rapid boil
which is required of the tougher, dryer "flinty" starches found in grains. Fill the
cooker with water and add the starchy material slowly. Heat the grain (and malt) to
62-63 C for 45 min to 1 hour (stir occasionally), using 4.5L water per kg grain, then
strain out the grains (use a kitchen sieve), keep the liquid (the wort/mash). When due
to separate the grains from the liquid (lautering), raise the temperature to 75-77 C. At
this "mash-off" temperature the wort viscosity is favourable for quick & complete
separation, enzymes are mainly inactive, and bacterial action is precluded.
3. Primary Fermentation. Measure the specific
gravity and sugar content value for each of the
starting substrates with a hydrometer. Inoculate
each bottle with 20 ml of the starter yeast culture
per liter of mash prepared in the previous steps.
Plug the mash bottle with a rubber stopper. A
piece of tubing is extended from the stopper to
provide a vent for the evolved carbon dioxide. The
other end of the tubing is dipped in water in a
small test tube taped to the bottle. The water
prevents the entry of oxygen, which alters the
metabolism of the yeast and spoils the wine. At
the same time, the volume of carbon dioxide can
Figure 5.1. Fermentation setup
be monitored if it did not escape. See Figure 5.1.
(Image taken from http://fileserver.net4. Ferment at room temperature for one week.
texts.com/asset.aspx?dl=no&id=22379)
5. Secondary Fermentation. At the end of one week,
decant the fermentation broth from the bottle to clean individual temporary
containers.
17
6. Measure the sugar content for each of the substrate with a hydrometer. Estimate the
alcohol content from the difference in the present sugar content value and the initial
sugar content value.
7. Discard the sediment and wash each bottle with water.
8. Pour the broth back into the cleaned bottle. Put back the cleaned assembly of rubber
stopper and rubber tubing.
9. Ferment slowly for another 4-6 weeks.
10. Measure the sugar content values as before when it is ready for consumption.
1. What is/are the main constituent of the raw material you used?
2. What happened during fermentation? Were all the sugars converted into alcohol?
How were you able to say so?
3. How much CO2 was produced? How is this related to the change in the amount of
sugar before and after fermentation?
4. What is the proof of the alcoholic beverage that you have produced? What is its
identity?
Comment on ways to improve the experiment.
References
http://www.uq.edu.au/_School_Science_Lessons/topic17.html#17.3.0 [Retrieved: 25 August 2015]
Cornelius S. Ough, Chemicals used in making wine, C&EN, January 5, 1987.
http://www.totalwine.com/eng/guide-to-wine/fermentation.cfm [Retrieved: 26 August 2014]
http://www.aromadictionary.com/articles/winefermentation_article.html [Retrieved: 26 August 2014]
http://running_on_alcohol.tripod.com/id20.html [Retrieved: 26 August 2014]
http://homedistiller.org/grain/wash-grain/mashing [Retrieved: 26 August 2014]
18
EXERCISE 6: PREPARATION OF CHEESE

Date started: _________________
Date due: ____________________

INTRODUCTION
Cheesemaking consists of three steps: the precipitation of casein into curds, the
concentration of the curds, and the ripening or aging of the curds. A wide variety of foods
such as yoghurt, sauerkraut, cheese, beer, wine, bread, soy sauce and coffee beans, owe
their production and characteristic flavours and textures to the fermentative activities of
micro-organisms. Micro-organisms involved in fermentation reactions include molds,
yeasts (bread, beer and wine) and a group of bacteria collectively referred to as Lactic
acid bacteria. Such micro-organisms use the sugars in food as a source of energy. Lactic
acid causes the pH of the food to drop, which kills the pathogenic bacteria and inhibits the
growth of many of the common spoilage micro-organisms. Other chemicals produced
give the foods their distinctive flavour and odour.
In this experiment, students will learn the basic processes involved in the
preparation of cheese.
A. Equipment
Measuring cup
Pipet or medicine dropper
Hot plate
Thermometer
Spatula
Muslin or chux or cheese cloth
Balance
Cooking pots
Small bowl or plastic cup
B. Reagents
Pasteurized milk, whole, (to be
supplied by the student) - Use
fresh farm milk if you can as this
will give best results.
If
purchasing milk use full cream
pasteurised milk. Homogenized
milk because of all the processes
that it has gone through does not
produce the same rich and tasty
cheese. Skim milk can be used

but frequently to obtain a firmer,
richer curd you will have to add
in some cream. Soy milk and
UHT milk can produce cheese
that does not require rennet. You
can also use other milk types
such as almond milk, coconut
milk.
Butter milk or lactic acid
producing strains (to be supplied
by the student)
Vinegar or lemon juice (20mL
per 400mL of milk)
Distilled water
Calcium chloride
Sodium chloride (table salt)
Optional: food coloring and herbs
such as garlic, parsley, chives,
dill, etc.
Cheese wax or beeswax
19
METHODOLOGY
1. Setup the double boiler. You can use what you have in the kitchen but make sure that
the inner pot is stainless steel. The reason that you use a double boiler is to prevent
scalding of the milk.
2. Place the pasteurized milk in the inner pot. Add one ml of buttermilk per 100 ml of
milk. After 30 minutes, raise the temperature of the mixture to 32C with constant
stirring, and add artificial coloring (if there is any) to the mixture prior to curdling.
Record any changes in the milk.
3. Add the vinegar or lemon juice and stir to mix. Let it stand for 30 minutes to allow
coagulation to proceed. Do not disturb the coagulation process in the containers;
otherwise, the curds will be broken into pieces too small to filter efficiently with
cheese cloth.
4. After curd formation, break up the curds with a stirring rod or spatula and drain the
whey through layers of cheese cloth. Pick up the cheesecloth by the corners. Do not
squeeze any liquid from the curds that will make the cheese dry and tough.
5. Use a spatula to scrape the cheese curds off the cheesecloth into a small bowl or
plastic cup. If your curd is not "firming up" and this can happen if you have used
homogenized, long life or UHT milk, you can add in some calcium chloride which
boosts the calcium content of the milk and helps to produce a firmer, tighter curd.
6. Dispose off the whey.
7. Taste your cheese. Weigh the amount of curd obtained in its wet state and
approximate the yield. Record your observations.
8. After the curd is separated from the whey, salt, seasoning, and other curing and
flavoring ingredients may be added. The herb flavors may take about 15 minutes to
penetrate through the cheese.
9. It is now ready for consumption, or it may be left to age in a controlled cool
environment (2-13C). Although a higher temperature promotes faster curing, there is
also a higher chance of spoilage due to undesirable microbial activities at elevated
temperatures. Prior to aging, the cheese block is usually wrapped tightly to exclude air
and microbial contaminants from entering and spoiling the cheese. One way to
accomplish this is to dip the cheese block in a pot of melted cheese or beeswax.
10. While the cheese dries begin melting the wax. To be most successful at preventing
mold growth, the wax needs to reach a temp of 225-2400F and the cheese dipped for
at least 6 seconds. You really need to control the temperature because if the wax gets
hotter it might reach its flash point and catch on fire.
11. After heating the wax, turn the burner off and place a piece of foil on the stove or
work surface to catch the drips (much easier to clean up).
12. Work cautiously and make sure you have a good grip on the cheese before dipping.
Dip the top of the cheese, let that cool, then dip the bottom. Once these surfaces are
cool rotate one half of the cheese edge in the wax, let that cool, and then wax the other
half. When finished, simply allow the wax to cool and then store it covered on the
shelf to keep dust out.
13. During the aging process, many complicated microbial and chemical actions continue
to take place in the cheese block. These reactions are not well characterized; thus,
20
cheese making is still an art rather than a science. Depending on the technique
employed, this final aging process takes anywhere from 2 weeks to 6 months.
14. If you find mold growing on a waxed cheese, either the surface was not heated hot
enough during the waxing to kill off the mold (wax too cold) or a small pinhole was
left for mold to enter. If very serious, this mold should be taken care of ASAP by
removing the wax, brushing or scraping the mold from the surface, and giving the
cheese a good wiping/scrubbing (depending on how serious) with a cloth soaked in
saturated brine. The cheese should be allowed to dry and then re-waxed.
SAFETY PRECAUTIONS
Safety glasses or goggles must be worn in the laboratory at all times. All work surfaces
must be cleaned and free from laboratory chemicals. It is advised to cover all work areas
with aluminum foil or a food-grade paper covering. All glassware and apparatus must be
clean and free from laboratory chemicals. Special glassware and equipment, reserved
only for food experiments is recommended.
Wax when heated will reach a point where vapors accumulate and may ignite with life
threatening results.
GENERAL HYGIENE
Sterilise everything before use. You should have clean working surfaces and equipment
including hands. You can sanitise equipment using 12 mililitres bleach to one litre cold
water. If you go off and do something else while waiting, remember to sanitise your
hands before you recommence cheesemaking.
Wear a long apron as cheesemaking can be messy. Hot curd cheese like mozzarella
requires stretching so purchase some rubber gloves otherwise you will burn your hands
and also watch out for boiling curd and whey landing on your feet. It is not sensible to
wear open toed shoes when making cheese. If you want to tie or cover your hair this is
also a sensible thing to do.
1. Report your observation of this experiment and discuss the effect of pH on the yield
of the curd. You may try out other types of processed milk such as nonfat milk and
powdered milk. Are they suited for cheese making?
2. What is/are the main constituent of the raw material you used? Give a list of the
chemical components found in milk.
3. What happens during curdling of the milk?
4. Why is the coloring added before coagulation instead of afterwards?
5. What happens during aging of cheese?
6. Milk spoilage can be detected visually by the presence of coagulated curd. Identify
the chemical mechanisms responsible for spoilage of milk. Are these
chemicals/enzymes produced by contaminant microbial actions? Is the curd resulting
from spoilage the same as that used in cheesemaking? If they are the same, why
would you consume cheese but not spoiled milk?
21
References
Prins, J., Microbial rennet, Process Biochem., May, 1970.
Robinson, R.K., Dairy Microbiology, Vol. 2, Applied Science Publishers, New Jersey, 1981.
Richmond, H.D., Dairy Chemistry, A Practical Handbook, Charles Griffin & Co., London, 1930.
Constituents of milk: Jenness, R. and Patton, S., Principles of Dairy Chemistry, John Wiley, 1959, p3.
http://www.wikihow.com/Make-Cheese-at-Home [Retrieved: 2 September 2014]
http://www.curdsandwhey.co.nz/how-to-make-cheese [Retrieved: 2 September 2014]
http://www.eng.umd.edu/~nsw/ench485/lab1.htm [Retrieved: 2 September 2014]
http://www.chymist.com/cheese.pdf [Retrieved: 2 September 2014]
http://practicalbio.blogspot.com/2011/12/easy-enzyme-experiment-rennet-and.html
[Retrieved:
2
September 2014]
http://sciencenetlinks.com/student-teacher-sheets/cheese-making-project-instructions/
[Retrieved:
2
September 2014]
http://www.instructables.com/id/Kitchen-laboratory%3a-Proteins-and-Cheese-making/?ALLSTEPS
[Retrieved: 2 September 2014]
http://www.ift.org/~/media/Knowledge%20Center/Learn%20Food%20Science/Experiments%20in%20Foo
d%20Science/TeacherGuideEMULSIFIERS.pdf [Retrieved: 3 September 2014]
http://www.instructables.com/id/Kitchen-laboratory%3a-Proteins-and-Cheese-making/?ALLSTEPS
http://www.culturesforhealth.com/how-to-make-cheddar-cheese-recipe [Retrieved: 3 September 2014]
http://www.nzifst.org.nz/careers/secondaryresources.asp [Retrieved: 3 September 2014]
https://faculty.washington.edu/chudler/pdf/tastetg.pdf [Retrieved: 3 September 2014]
http://msucares.com/pubs/publications/p2469.pdf [Retrieved: 3 September 2014]
https://www.okcareertech.org/educators/cimc/new-products/clusters/science-technology-engineering-andmathematics-cluster/pdf-files/enzymesandfoodprep.pdf [Retrieved: 3 September 2014]
http://www.accessexcellence.org/pizza/pdf/fcbook.pdf [Retrieved: 3 September 2014]
http://nordicfoodlab.org/blog/2012/03/lactic-fermentation [Retrieved: 3 September 2014]
http://sciencenetlinks.com/media/filer/2012/01/24/cheeserecord_actsheet.pdf [Retrieved: 3 September
2014]
http://www.fssai.gov.in/Portals/0/Pdf/15Manuals/FOOD%20ADDITIVES.pdf [Retrieved: 3 September
2014]
http://www.slideshare.net/tammyhulse/basics-of-hard-cheese [Retrieved: 3 September 2014]
http://www.cheesemaking.com/WaxingCheese.html [Retrieved: 3 September 2014]
http://www.cheesemaking.com/store/pg/245-FAQ-Aging-Cheese.html [Retrieved: 3 September 2014]
http://essentialstuff.org/index.php/2011/06/06/Cat/cheese-making-waxing-the-round/
[Retrieved:
3
September 2014]
http://www.rifst.ac.ir/Portals/3/file/book/Food%20Analysis%20Laboratory%20Man
ual,%202nd%20ed.%20%28Food%20Science%20Text%20Series%29-S.%20Suzanne%20Nielsen144191.pdf [Retrieved: 3 September 2014]
http://www.cheesemaking.com/WaxingCheese.html#Anchor-49575 [Retrieved: 3 September 2014]
http://curd-nerd.com/waxing-cheese/ [Retrieved: 3 September 2014]
22
EXERCISE 7: PRODUCTION OF PAPER

Date started: _________________
Date due: ____________________

INTRODUCTION
Paper is so essential to writing that we couldn't do without it, and yet it was not
invented until several millennia after the invention of writing. Writing was invented about
5500 years ago by Sumerians in ancient Mesopotamia. As a medium for their texts,
Sumerians used clay tablets. Shortly after the Sumerians, ancient Egyptians developed
their own writing and invented the papyrus. Papyrus takes its name from the plant from
which it was obtained. They extracted thin strips from the spongy stem of this plant that
they placed side by side, partly overlapping. Subsequently, over the first layer of strips,
they superimposed a second layer, placing the strips transverse to those below. The
natural glues present in this plants tissue insured the adhesion of the strips. After its
invention in 105 A.D., the Chinese came up with large quantities of paper made from rags
and vegetable fibers extracted from hemp, bamboo, mulberry, and willow. In search of a
substitute to rags, in 1719 a Frenchman, who had observed wasps while building their
nests, suggested trying wood to make paper. The trials that were carried out were a
success and since then wood has become the main raw material for producing paper.
In principle, paper is made by: 1) pulping, to separate and clean the fibers; 2)
beating and refining the fibers; 3) diluting to form a thin fiber slurry, suspended in
solution; 4) forming a web of fibers on a thin screen; 5) pressing the web to increase the
density of the material; and 6) drying to remove the remaining moisture. To render it
suitable for writing or printing, it is necessary to lower the absorption of ink which
otherwise would spread. For this purpose, animal or synthetic glues are added to it. To
make paper less porous, more compact and even brighter, it is coated. Coating consists of
adding very fine mineral powders such as kaolin, calcium carbonate, talc, fossil flour, and
an appropriate adhesive such as casein or other types of glue. The sheet passes through
rollers which press it with force (calendering) and comes out bright. The goal of this
laboratory activity is to prepare paper from fibrous raw material and recycle used paper.
Small pieces of several types of used
paper (brown paper bag, newspaper,
tissue, etc.)
Fibrous raw material (i.e. bagasse)
Water
Spatula
Flat sponge
Muslin or chux or cheese cloth or
rags
Filled soft drink bottles to be used as
rolling pins
Drying boards
Wooden deckle
Egg Beater or mortar with pestle
Cooking pots
Hand lens or magnifying glass
Graduated cylinder or measuring cup
Hot plate
Thermometer
Balance
Sink
23
METHODOLOGY
1. Dry the bagasse/wood chips in the oven at preset temperature of 135 0C for 45
minutes. There is no need to perform this step if material is sufficiently dry.
2. Fiber Separation.
For recycled paper: It is necessary to turn the paper into pulp first before recycling it
into paper again. Here, mechanical pulping process will be used. First, put hot tap
water in a pot. Cut the scraps of paper into small pieces and add it to the hot water.
Start beating the mixture until it is mushy or pulpy. Record in your data table the time
the beating is started. After beating, a mild detergent can be used to clean the pulp;
however, make sure to rinse all of the detergent with water. Drain the water using
filter or cheesecloth.
For fibrous material: Use chemical pulpingKraft pulpingprocess. Place the dried
bagasse/fibrous material in a pot then add cooking liquor* using a fiber/liquid ratio of
1:10 mass ratio. Cook for 2 hours. Make sure to wear PPE prior to this step. Cool to
room temperature. Filter the pulp from the brown liquor by decanting. Rinse pulp
with water. The pulp is now ready for bleaching and further processing.
*Cooking liquor concentration is 12.5%wt solution of NaOH, Na2S and Na2CO3.
Typical analysis of solids: 58.6% NaOH, 27.1% Na2S and 14.3% Na2CO3.
3. Bleaching or Brightening. Since the raw pulp (brown stock) still contains an
appreciable amount of lignin and other discoloration, it must be bleached to produce
light colored or white papers preferred for many products. Bleaching is normally done
in several stages (multistage bleaching). You may use sodium bisulfite, calcium or
sodium hypochlorite (i.e. Zonrox), hydrogen or sodium peroxide for this purpose.
4. Papermaking. The bleached or unbleached pulp may be further beaten and refined to
cut the fibers and roughen the surface of the fibers (fibrillate).
Transfer the pulp into the sink with covered holes. Dilute it with tap water to make a
thin mixture normally containing less than 1 percent fiber. Dip the wooden deckle
into the sink. You may use your hands to cover it with the pulp and spread it out
evenly over the screen. Hold on to the frame with both hands and pull it straight up
out of the sink. Shake it very gently so the extra water drips back into the sink. You
may use a sponge to soak up even more water from under the screen while you keep
holding the frame flat. Set the frame on the stack of newspapers and rag, then press
another rag over the top of your sheet of paper and carefully peel the paper off. Lay
the rag with the sheet of paper on it flat on the counter to dry. When it is completely
dry, you can easily peel it off of the rag.
If your new sheet of paper rolls up when it dries, you can iron it flat using the iron's
lowest heat setting. Other things can be added to the pulp, like sizes to make the paper
less absorbent. Sizing can also be brushed or sprayed on the paper after it has dried.
24
Starch and gelatin were used traditionally, but these can sometimes attract insects and
mold. Methylcellulose is often used today to size hand-made paper. Lastly, test your
paper by writing on it.
NOTE: Paper properties include chemical properties (such as color, ph) & physical
properties (such as opacity, density, porosity, texture, strength, dimensional stability,
etc.)
SAFETY PRECAUTIONS
Put on safety goggles and a lab apron before starting the procedure. Also use care when
operating the beater/blender. Make sure your hands are dry when handling the
beater/blender or when plugging it in. Prepare MSDS for each of the chemicals used.
1. Look at each of the different types of paper you've collected with a magnifying glass.
Do you see the little hairy-looking pieces on the surface of the paper? Those are
called fibers. Do they all look the same? Are some longer or fatter than others? How
do the fibers of your paper and the commercial copy paper or newspaper differ? Why
do you think these differences occur?
2. Compare and Contrast. How did your piece of recycled paper differ from those of
your classmates? How can you explain these differences?
3. Use Models. Research more informationon the Internet, or in reference materials
about the process used to recycle paper commercially. How do the steps you followed
in this activity differ from the commercial process?
4. Apply Concepts. How might a factory that makes recycled paper ensure that every
sheet of paper has the same qualities, such as uniform texture, thickness, and color?
5. Extension. Research information about the recycling program in your community.
Suppose you are in charge of a campaign to raise awareness about the recycling
program and encourage people to participate. You decide to use a minimum amount
of new paper to make flyers, posters, or pamphlets. How could you do this? How
could you promote the program without using additional paper?
References
Venditti, R. Handsheet Preparation. <http://cnr.ncsu.edu/fb/extension/documents/handsheetmaking.doc>
Papermaking Lab 1. http://www.sewanee.edu/chem/Chem&Art/Detail_Pages/Laboratory/Papermaking
/Papermaking_Lab_1_07.htm [Retrieved: 9 September 2014]
Avila, B. Paper Making Science Project. http://www.hometrainingtools.com/a/paper-making-scienceproject-for-elementary [Retrieved: 9 September 2014]
Experiment 4: Recycle Paper. http://www.eh.uc.edu/cares/kids/games/images/RecyclePaperExperiment.pdf
Dianne van der Reyden. Teaching with Paper-Making. http://www.si.edu/mci/downloads/RELACT/
teaching_with_papermaking.pdf [Retrieved: 9 September 2014]
Pictures of the fabrication of papyrus. http://www.museolibroantico.com/corso_libro_antico.html
25
Chiparus,
O.
(2004).
Bagasse
Fiber
for
Production
of
Nonwoven
Materials.
http://etd.lsu.edu/docs/available/etd-02262004-111054/unrestricted/Chiparus_dis.pdf?q=bagasse-products
Ban, W., Wang, S., Lucia, L. The relationship of pretreatment pulping parameters with respect to
selectivity: optimization of green liquor pretreatment conditions for improved kraft pulping.
http://www4.ncsu.edu/~dsargyro/documents/PretreatmentPulpign ParametersandSelectivity.pdf [Retrieved:
10 September 2014]
Chapter 2: The Pulp and Paper Making Processes.
https://www.princeton.edu/~ota/disk1/1989/8931/893104.PDF [Retrieved: 10 September 2014]
Ragauskas, A. Basics of Kraft Pulping & Recovery Process.
http://ipst.gatech.edu/faculty/ragauskas_art/technical_reviews/Kraft%20Pulping%20and%20Recovery%20
Process % 20basics.pdf [Retrieved: 10 September 2014]
26

1601 - Indus Chem Lab Manual

Загружено:

Сведения о документе

Исходное описание:

Оригинальное название

Авторское право

Доступные форматы

Поделиться этим документом

Поделиться или встроить документ

Параметры публикации

Этот документ был вам полезен?

Это неприемлемый материал?

Авторское право:

Доступные форматы

1601 - Indus Chem Lab Manual

Загружено:

Авторское право:

Доступные форматы

Department of Chemical Engineering

GENERAL INFORMATION ABOUT

Chemistry of Oils, Fats

Short revisit of needed

and Wax Processing

of fats, oils and waxes

Lec3: Case Study/

Lec8: Problembased learning

Identify the major

Hydrogen Peroxide and

Midterm Processing and

and the reactions

Industrial Acids and

Lab10: Plant visit/

Lab11: Plant visit/

Web and Other Learning Resources

Class standing requirements (short quizzes, seatworks, assignments and oral

Average of class participation (board

Average of homeworks and projects

Grade conversion table

*INC grade is released if a major

Average of homeworks and projects

minimum. INC grades are to be

Student is at ease with

Student maintains eye

Rubric B: Written Report (adapted from http://www.sdst.org/shs/library/resrub.html)

Student(s) posed a thoughtful,

Student(s) posed a focused

Student(s) relied on teachergenerated questions or

Student(s) showed little

research. Product does

Rubric C: Laboratory Report

Total Points Earned

Rubric D: Self and Peer Performance Evaluation (during Laboratory)

GUIDELINES FOR SAFETY IN THE

21. Do not smell directly any chemical being heated.

REVISION HISTORY AND ACKNOWLEDGEMENT

General Information About The Laboratory ...

Guidelines for Safety in the Chemical Engineering Laboratory

Revision History and Acknowledgement ...

I. CHEMISTRY OF OILS, FATS AND WAX PROCESSING

II. CHEMISTRY OF FLAVORS AND FRAGRANCES

III. CHEMISTRY OF SURFACTANTS AND THE MANUFACTURE OF

IV. CHEMISTRY OF SACCHARIDES

V. FERMENTATION PROCESSES AND THEIR APPLICATION

VI. PULP AND PAPER

EXERCISE 1: COCONUT OIL EXTRACTION

Date due: ____________________

EXERCISE 2: EXTRACTION OF ESSENTIAL OILS

Date due: ____________________

(Image taken from 3

EXERCISE 3: PREPARATION OF SOAP

Date due: ____________________

Graduated cylinder (or measuring

dissolved in the solvent. Caution:alcohol is highly flammable. Wear personal

EXERCISE 4: REFINING OF SUGAR

Date due: ____________________

EXERCISE 5: ALCOHOLIC FERMENTATION

Date due: ____________________

EXERCISE 6: PREPARATION OF CHEESE

Date due: ____________________

cheese. Skim milk can be used