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CHEMICAL AND ENVIRONMENTAL ENGINEERING 125
Analytical Methods for Chemical & Environmental Engineers Laboratory

DEPARTMENT OF CHEMICAL &


ENVIRONMENTAL ENGINEERING
BOURNS COLLEGE OF ENGINEERING
UNIVERSITY OF CALIFORNIA, RIVERSIDE

Laboratory Manual

ANALYTICAL METHODS FOR CHEMICAL AND ENVIRONMENTAL ENGINEERS LABORATORY

Laboratory Manual

UC Riverside, 2014
Bourns College of Engineering
Department of Chemical and Environmental Engineering
Riverside, CA 92521

Table of Contents
CHAPTER

CHAPTER

Laboratory Exercises, Organization,

Experiment #1 Accurate volume

and Scheduling

measurement by using burets and pipet

18

Laboratory Preparation

Experiment #2 - Identification of a substance

Personnel

by acid-base titration

21

Experiment #3 - UV-Vis SpectroscopyCHAPTER

Determination of the cobalt and Nickel

Laboratory Conduct

concentrations

22

General Rules

Experiment #4 - AAS

23

Care and Use of Laboratory Equipment

Experiment #5 - HPLC

24

Care and Use of Chemical Reagents

Experiment #6 - GC

26

CHAPTER

CHAPTER

General Considerations

11

Guidelines for lab report submission and

Sources of Errors

12

grading policy

Uncertainty Analysis

13

Statistical Analysis of Data

14

Population Statistics

14

Graphical Analysis

15

27

I N T R O D U C T I O N

Chapter

INTRODUCTION
What is the purpose of Analytical Methods for Chemical and
Environmental Engineers Laboratory

he course, Analytical Methods for Chemical and Environmental Engineers


Laboratory, CHE & ENVE 125, is designed to provide an introduction into
instrumental methods and their use in chemical and environmental
engineering.

To avoid crowded lab conditions and give each student as much hands-one experience
as possible, each lab section is limited to 20 students. Students will work in groups of
two/four. Groups will stay together throughout the quarter. It is important that the
members of the group work together to complete the laboratory exercises and submit
written reports in a time efficient manner. It is strongly recommended that each group
review the informational handouts together prior to doing the lab work, and determine
work tasks before conducting the lab. During each session each student should record
the experimental data in her/his laboratory notebook.
All lab reports are submitted as group lab reports. Write-ups are due at 5 pm one
week after the lab is conducted and are to be given to the laboratory instructor
(TA). Requirements for the lab write-ups will be discussed later in this chapter.

Laboratory Exercises, Organization, and


Scheduling
There are a total of 7 different laboratory exercises for CHE/ENVE 125. The two
labs on basic laboratory measurement techniques and five labs on instrumental analysis
will be conducted over ten weeks.

I N T R O D U C T I O N

The two laboratory measurement technique laboratories are:


Lab No.
1
2

Topic

Accurate volume measurement by using burets


and pipet
Identification of a substance by acid-base titration

The four instrumental analysis laboratories are:


Lab No.
3
4
5
6

Topic

UV-Vis Spectroscopy-Determination of the


cobalt and Nickel concentrations
Atomic Absorption Spectroscopy (AAS)
High Performance Liquid Chromatography
(HPLC)
Gas Chromatography (GC)

As noted previously, there will be two/four students per lab group. Unless a student
withdraws from the class, the composition of each lab group will remain fixed for the
entire quarter. During the first week of the quarter, groups will be determined and
assigned a number.
If difficulties arise within a group, please communicate them to the faculty member in
charge. REMEMBER, HOWEVER, AN IMPORTANT CHARACTERISTIC
THAT EMPLOYERS ASK ABOUT IS HOW WELL A PROSPECTIVE
EMPLOYEE CAN WORK AS A TEAM. In a company you will not be able to pick
the people you work with. You must be able to overcome personal idiosyncrasies to
get the job done - period.
The general laboratory schedule will be:
Week
No.
1
2
3
4
5
6
7
8
9

Date

Task

January 6, 7, 8
January 13, 14, 15
January 20, 21, 22
January 27, 28, 29
February 3, 4, 5
February 10, 11, 12
February 17, 18, 19
February 24, 25, 26
March 3, 4, 5

Introduction, lab safety training


Laboratory measurement technique
Laboratory measurement technique
Instructions on use of instruments
Instrumental analysis laboratory
Instrumental analysis laboratory
Instrumental analysis laboratory
Instrumental analysis laboratory
Presentation

I N T R O D U C T I O N

The schedule for measurement technique experiments for all groups is as follows:
Lab
No.
1&
2

Topic

All Groups

Laboratory
measurement
techniques

1/13 to
1/22

1/13 to
1/22

1/13 to
1/22

1/13 to
1/22

Instructions on
use of instruments

1/27,
1/28 &
1/29

1/27,
1/28
&1/29

1/27,
1/28 &
1/29

1/27,
1/28 &
1/29

The schedule for instrumental analysis experiments is as follows:


Lab
No.

Instrument

UV-Vis

AAS

HPLC

GC

Group
A&E
2/3,
2/4 &
2/5
2/24,
2/25 &
2/26
2/17,
2/18 &
2/19
2/10,
2/11 &
2/12

Group
B&F
2/10,
2/11 &
2/12
2/3, 2/4
& 2/5
2/24,
2/25 &
2/26
2/17,
2/18 &
2/19

Group
C&G
2/17,
2/18 &
2/19
2/10,
2/11 &
2/12
2/3, 2/4
& 2/5
2/24,
2/25 &
2/26

Group
D&H
2/24,
2/25 &
2/26
2/17,
2/18 &
2/19
2/10,
2/11 &
2/12
2/3, 2/4
& 2/5

When you find out what your lab group number is - write it down here.
MY LAB GROUP NUMBER IS ________.
MY INSTRUMENT ANALYSIS GROUP LETTER IS ________.

Laboratory Preparation
Laboratory notebook. Notes and data should be recorded with an ink pen in a
permanently bound laboratory notebook. The most useful notebook is one that
has pages that makes graphing easy. Students should purchase one before the
beginning of the first exercise and use the same notebook for each experiment.
Record pre-experiment notes, changes from standard procedures made during

I N T R O D U C T I O N

the course of the experiment, data, preliminary data reduction (for example,
checks of a calibration curve to make sure an instrument is operating correctly),
and any other observations that you may feel are interesting and noteworthy.

Why is it important to record information in a permanently bound notebook?


Loose papers and pages in spiral bound notebooks are easily lost. Further, a
permanently bound notebook is a journal of your in the laboratory. Journals are
extremely important when legal issues such as patents and lawsuits come about.
The time and activities associated with the experiment are entered sequentially.
Thus, there can be no question of whether information was added at a time
other than when the experiment was conducted and that the information was
indeed collected from the experiment and not another source.
Each laboratory session requires considerable preparation.

Students are expected


to be familiar with the general procedures before coming to the lab session and should
have her/his laboratory notebook ready to enter data. DATA SHOULD NOT BE
RECORDED ON SCRAP PIECES OF PAPER. The TAs will not be responsible
for providing data for the experiments or making sure students have collected all of the
necessary data.
The laboratory manager and TAs will generally check that all of the equipment is in
good working order and they will make sure that all necessary gases and/or solutions
are available for the labs. The TAs will demonstrate the proper used of the equipment.
However, other than ensuring that the students carrying out the lab exercises in a safe
manner, the TAs will be there primarily to answer questions, not run the instruments
for the lab exercise.

Personnel
Class Instructor:

The professor for the class is Dr. Ashok Mulchandani, his office
is in B317, his phone is (951) 827-6419, and his email address is adani@engr.ucr.edu.
Laboratory Manager

The Chemical & Environmental Engineering Laboratory Manager is Kathy Cocker.


Her office is in A229 Bourns Hall and her email address is ksmihula@engr.ucr.edu.
Laboratory Instructors

The TAs for Winter 2015 are Tingjun Wu (email address: twu020@ucr.edu), Justin
Neal (email address: jneal002@ucr.edu) and Trupti Terse (email address:
trupti.terse@email.ucr.edu).
TA Office hours: TBA

L A B O R A T O R Y

S A F E T Y

A N D

P R O T O C O L

Chapter

LABORATORY SAFETY AND PROTOCOL


What to do and what not to doabove all use common sense!
The Chemical and Environmental Engineering Programs are privileged to have
excellent teaching and research laboratories in Bourns Hall. Rooms B108, B134 and
B235 are the principal wet-lab teaching laboratories. B314, B316, B318, B328, B328A,
B350 and B334 are the research laboratories areas. The general research topics and
faculty responsible for the research labs are as follows:

B312 Bourns Biotechnology research laboratory Dr. Mulchandani


B314 Bourns - Nanobiotechnology - Dr. Ashok Mulchandani
B316 Bourns - Genetic engineering - Dr. Ian Wheeldon
B318 Bourns Dr. Mark R. Matsumoto
B328 Bourns - Dr. Phillip Christopher ; Dr. Xin Ge; Bacterial adhesion
laboratory - Dr. Sharon Walter

B350 Bourns-Nano electrochemical system laboratory Dr. Nosang V.


Myung

B334 Bourns - Cold room (general support)


If you are interested in working in any of these areas or with any of these faculty
members, students are encouraged to contact the various faculty members.

LABORATORY CONDUCT
Proper conduct of everyone in the laboratories is important not only for the efficient
and congenial operation of the labs, but also for the safety of all involved. This
conduct applies to ALL STUDENTS - undergraduate, graduate, and postdoctoral.
ALL STUDENTS ALSO NEEDED TO COMPLETE AN ONLINE

L A B O R A T O R Y

S A F E T Y

A N D

P R O T O C O L

SAFETY TRAINING ON OR BEFORE JANUARY 15, 2013. Student can go


through the following link to complete their online safety training.

http://ehs.ucr.edu/training/online/lso/indexlms.html

General Rules
Please read these
rules thoroughly.
They are very
important in
ensuring that
students have a
safe lab
experience.

Clothing and shoes: Closed toe shoes and pants that cover the ankles are mandatory.
Open toe sandals are not adequate protection from chemical spills. Spills and
accidents can (and do) happen. Students should not wear clothes that they are worried
about damaging and must purchase a lab coat from the bookstore for participation in
class labs. Clothing is readily damaged as a result of chemical spillage and splashing,
particularly from strong acids, bases, and redox chemicals. As an added precaution
students should wear a chemical resistant apron when handling strong
acid/base/solvent chemicals.
Safety Goggles: CHEMICAL SAFETY GLASSES OR GOGGLES MUST BE
WORN AT ALL TIMES IN THE LABORATORY. If you wear eyeglasses, they
should have splash shields to protect against chemical splashing. Regular eyeglasses, by
themselves, are not adequate protection against chemical splashing. Also, certain
chemicals may ruin plastic lenses. It is recommended that students purchase a pair of
chemical safety glasses/goggles from the bookstore and reserve them for their personal
use when working in the laboratories.
Eyewash stations and showers: There is an eyewash and safety shower located in
the teaching and research laboratories. In addition, drench showers are located in
several of the research labs. Familiarize yourself with the location and use of these
safety items.
Eating and Smoking: Eating, drinking or smoking is not permitted in any of the
laboratories.
Animals and Pets: Animals and pets are not permitted in any of the laboratories.
Refrigerator and Ovens: Refrigerators, incubators, and ovens located in the
laboratories are not to be used for storing or preparing food.
Flames: Open flames should be placed in a fume hood if possible and always on a
non-flammable surface away from combustible material. Never leave open flames
unattended in the lab.
Chemical Spills: Small spills should first be neutralized: sodium borate for base spills
and sodium bicarbonate for acid spills. After neutralizing mop or sponge up spills
immediately. Large spills should first be contained with an absorbent material such as

L A B O R A T O R Y

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A N D

P R O T O C O L

vermiculite and then neutralized. Additional absorbent may then be added to take up
the neutralized liquid and picked up. A faculty member or the Laboratory Manager,
and Environmental Health and Safety (25528) should be notified when a large spill
occurs.
Volatile Organics: A fume hood should be used when using or dispensing a volatile
organic reagent. If the reagent is to be regularly used or dispensed for a project, as
additional protection, an appropriate respirator should be purchased, fitted, used, and
regularly maintained. Respirators should not be shared; they are to be purchased,
fitted, used, and maintained by one person. Environmental Health and Safety will fit
and test respirators free of charge.
Pipetting: NEVER pipet any solutions by mouth. Pipet with a pipet bulb or a
pipettor. After using any pipet, please place it in a pipet storer for subsequent washing
in a pipet washer.
Gas cylinders: Pressurized gas cylinders should be strapped or chained to a bench
top or wall. Before moving cylinders always remove regulators and screw on the cap.
DO NOT attempt to change regulators without prior training. Depending on the gas
type, regulator threading and connections vary to prevent mixing of incompatible
materials. Empty gas cylinders should be returned to the supplier as soon as possible.
Chemical waste disposal: Chemical wastes, spent and old reagents, and effluents
from bench-scale reactor systems SHOULD NOT BE DISPOSED INTO THE
FLOOR DRAINS OR SINKS! Before beginning your laboratory experiment, check
with a faculty member of the Laboratory Manager regarding proper disposal of
expected wastes. Environmental Health and Safety will collect and dispose of
hazardous wastes upon request.
Daily departure: Check your work area when you leave for the day to be sure
everything is clean and neat. If you are the last person in the room, check all sinks in
the room to make sure the tap water is turned off. Make a cursory glance around the
remainder of the laboratory to see if there are any major problems. If you are the last
one to leave for the day, please check each lab to see that all tap water is off, that there
are no major problems, and that all doors are locked. As you leave the laboratory
TURN OFF THE LIGHTS AND LOCK THE DOORS.

CARE AND USE OF LABORATORY EQUIPMENT


Many of the analytical instruments and much of the laboratory equipment in the
Chemical and Environmental Engineering Laboratories are commonly used for both
teaching and research. Therefore, it is imperative that each student use and maintain
instruments and equipment properly.

L A B O R A T O R Y

S A F E T Y

A N D

P R O T O C O L

BEFORE USING ANY ANALYTICAL INSTRUMENT

Read the instruction manual or obtain training by qualified personnel on the use, care,
and maintenance of the instrument. Please contact the Laboratory Manager
regarding instruction manuals or training.
Failure to use and maintain instruments properly will lead to poor laboratory results
and jeopardize the progress of important research projects. Students who use and
maintain of laboratory instruments and equipment improperly may be subject to
disciplinary action.
From time to time, students may experience problems when using some of the
analytical instruments. When problems occur, they should be discussed with the
Laboratory Manager. DO NOT ATTEMPT TO "FIX" THE INSTRUMENTS
WITHOUT CONSULTING WITH A FACULTY MEMBER OR THE
LABORATORY MANAGER.
Balances: Balances and their surrounding areas should be cleaned using a brush after
each use. Residual traces of reagents, liquids, etc. should not be evident. The
experiment of the next person using the balance may be ruined by your laziness and
lack of consideration.
pH Meters: pH meters are available in various laboratory rooms. They are not to be
moved from the room without permission from the Laboratory Manager or faculty
member. The pH probes should not be used in harsh solutions or solutions that may
foul the probe. After use, the probes should be rinsed and placed in a neutral buffer
solution for storage; pH meters should be placed in a stand-by mode.
Ovens and Furnaces: Convection ovens are primarily for reagent desiccating and
solids/moisture analyses, and are typically set at around 100 to 110oC. Muffle furnaces
are primarily used for volatile solids analyses and are set at around 550oC. Do not
adjust the temperatures of ovens or furnaces without consulting with the other users.
Autoclaves: In addition to small autoclaves located in several of the research
laboratories, a large autoclave for sterilizing glassware and culture media is located in
B358 Bourns Hall. Students needing to use this autoclave should consult with the
Laboratory Manager before use.
Fume hoods: The Chemical and Environmental Engineering Laboratories contain
two types of fume hoods: canopy (elephant trunk) and sash. Sash-type fume hoods
are to be used for making up strong acid/base reagents, dispensing volatile chemicals,
and performing digestions and extractions. When using sash-type fume hoods, the
glass screen should be lowered at all times, except when placing equipment and or
chemicals inside. Always prepare reagents with the glass screen lowered, wearing

L A B O R A T O R Y

S A F E T Y

A N D

P R O T O C O L

goggles at all times. DO NOT STORE EQUIPMENT, CHEMICALS OR


REAGENTS IN SASH-TYPE FUME HOODS. Canopy fume hoods are to be used
when hazardous volatile vapors may be emitted from a bench-scale laboratory
experiments that runs for long periods of time.
Dishwashers: There are various laboratory dishwashers located in the labs to be used
for glassware cleaning. Instructions for their use can be obtained from the Laboratory
Manager. Often, however, glassware will need to be washed by hand. When washing
glassware, etc. by hand always wear goggles and gloves. You may not know what
residual chemicals may be present in dirty glassware. Do not store dirty glassware
around the sinks. Wash them first before leaving them to dry around the sink. This
will prevent an accident occurring when someone else picks up the glassware.
WHEN USING CHROMIC ACID OR OTHER DILUTE ACID SOLUTIONS
TO WASH GLASSWARE, BE SURE TO CLEAN THE SINKS, FLOORS, AND
SURROUNDING AREAS THOROUGHLY. YOU MAY CAUSE THE NEXT
PERSON TO HAVE SERIOUS BURNS AS A RESULT OF YOUR
NEGLIGENCE!
Borrowing: Environmental Engineering laboratory instruments and large equipment
should not be moved from room to room. If there is a need to do so for your
research, obtain permission from a faculty member or the Laboratory Manager.
EQUIPMENT OR SUPPLIES OF ANY KIND MAY NOT BE BORROWED OR
REMOVED FROM THE LABORATORIES FOR USE BY OTHER
DEPARTMENTS WITHOUT FIRST FILLING OUT A DEPARTMENTAL
EQUIPMENT LOAN FORM. SEE THE LABORATORY MANAGER FOR
PERMISSION AND THE NECESSARY FORMS.
DO NOT LOAN
EQUIPMENT OR SUPPLIES TO NON-CHEMICAL/ENVIRONMENTAL
ENGINEERING FACULTY OR STUDENTS WITHOUT CONSULTING
WITH THE LABORATORY MANAGER.
CARE AND USE OF CHEMICAL REAGENTS

Dry chemicals are separated generally into two categories: organic chemicals and
inorganic chemicals. Strong liquid acids and bases are stored separately in cabinets
under fume hoods. Volatile liquids are stored in cabinets which have exhaust vent
built in to carry away any off-gases.
Labeling: When new reagents are received, either for general lab use or for a specific
project, mark each bottle or jar of chemical with the month and year received, and your
initials (e.g. Rec'd 10/96 MRM). Also mark the bottle or jar when the chemical is first
opened (e.g. Open 12/96 MRM). Use labeling tape (not masking tape) or adhesive
label. Grease pencil, or other non-permanent marker, is not acceptable; labeling
information is easily erased.

L A B O R A T O R Y

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A N D

P R O T O C O L

Dispensing: When weighing reagents, use an intermediate container. Carefully


dispense the approximate amount of reagent you'll need into the intermediate
container first, then transfer the reagent onto the weighing vessel or paper in the
balance. Do not return excess chemical (in the intermediate container) back into the
reagent bottles.
Strong Acids and Bases: Liquid acids and bases should be dispensed in a sash-type
fume hood. Carry acid/base bottles in the rubber acid/base carrier, or use a cart.
Never carry acid/base bottles by the handle or neck. When holding an acid/base
bottle, always have one hand under the base of the bottle. Wear goggles, apron and
gloves when dispensing and mixing strong acids or bases. Mix strong acids or bases in
a Pyrex or Kimax flask or beaker. Ordinary flint glass reagent bottles will crack from
the heat. Add the acid or base to water in small incremental amounts over time.
ALWAYS add concentrated acids or bases to water. NEVER add water to
concentration acids or strong bases!!
Storage and Labeling of Reagent Solutions: Reagent solutions should be prepared
using volumetric flasks or graduated cylinders. However, solutions should NOT be
stored in them. After a reagent solution is made, it should be placed in a clean,
appropriately sized reagent bottle. The reagent bottle should then be labeled with the
following information: contents, date of preparation, preparer's initials, project,
disposal date (date beyond which reagent should be discarded), and other special
warnings (e.g. flammable, volatile, extremely caustic, etc.). An example is: 0.1 M
Sodium Hydroxide, Caution, Corrosive, MRM, Prep. 11/1/14, Dis. after 2/1/15.
Improperly marked reagents must be assumed to be old and will be discarded.
Water: There are three kinds of water available in our laboratories:
Tap water: Water at the sinks is regular water from the municipal water supply.
However, because there are many chemicals in use and the possibility of backflushing
exists, all of the taps are marked, Industrial Water - Do Not Drink. If you want
drinking water, please use the drinking fountains near the lavatories.
Reverse osmosis (RO) water - This water is available from the special taps marked
DI at each sink. This water is very high quality and is adequate for most reagent
purposes.
Nanopure water - This water is made by taking RO water and passing it through
activated carbon, two mixed bed ion exchange columns, and a 0.2 micron filter. This
water is the highest quality water available in the Chemical and Environmental
Engineering laboratories, and should be used sparingly, for mixing high purity reagents
and standards, and for final rinsing of special glassware.

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D A T A

A N A L Y S I S

B A S I C S

Chapter

DATA ANALYSIS BASICS


Some form of analysis is required on experimental data. The analysis may be a
very simple qualitative assessment about an observed trend or it may involve
complex error analysis coupled with a statistical analysis to determine the
probability of true differences between experimental data sets.
While the ability to carry out experiments and collect data is important, the usefulness
of conducting experiments depends on careful analysis of the collected data. Without
analysis, an experiment is merely a work task. Data analysis can be used for a variety of
purpose such as determining 1) whether collected data are reasonable, 2) the
uncertainty associated with the measurements 3) whether significant differences in data
sets exist as a result of changed operating conditions, and 4) empirical mathematical
models for relationships between different parameters. However, the analysis of
experimental data is an acquired skill that improves (hopefully) with experience. One
of the purposes for this course is that students begin to develop these skills.

General Considerations

A good outline that can be used for experimental data analysis has been developed by
Holman1 (1994).
1. Examine data for consistency. Are the measurements reasonable? This basic question
is the common sense approach to experiments. A simple example is when you fill
up your car with gasoline, you expect your gas gage to read Full right after. If it
doesnt, you suspect something is wrong like the gage is broken, your gasoline tank
leaked, or the pump wasnt working correctly.
This same logic applies to engineering experiments. When you bubble pure
oxygen gas through water that is not saturated with oxygen, you would expect that
dissolved oxygen concentration to increase, not decrease or stay the same. Why do
you know this? Based on mass transfer considerations (of course!).

Holman, J.P. Experimental Methods for Engineers, 6th ed., McGraw-Hill, Inc., San Francisco, 1994.

11

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B A S I C S

To use this common sense approach it is important that the experimenter be


familiar with the expected trends/readings based on theory and/or past
experience. You dont want to continue doing an experiment if you are collecting
bad data. If you know beforehand what to expect, this type of situation can be
avoided. The more thorough the understanding of what is expected based on
theory and/or experience prior to the start of an experiment, the more likely it is
that the experiment will be successful.
2. Perform a statistical analysis of data where appropriate. When measurements are repeated
several times, statistical parameters such as mean, median, and standard deviation
are useful in evaluating the level of precision for a particular measurement, and
level of confidence for a given data set.
3. Estimate uncertainties in the results. All instruments that measure something have an
uncertainty associated with them. For example, when a thermometer reads 100oC,
is it accurate to 1oC or 0.1oC. If the temperature reading is used in conjunction for
another parameter such as heat content, then the temperature uncertainty carries
over to heat content as well. Generally, these types of uncertainties can be
estimated before the experiment is conducted.
4. Anticipate results from theory. The theory or theories relevant to the experiment
subject should be carefully reviewed to determine what trends may be expected
before the experiment takes place. This step is particularly important in
determining an appropriate graphical presentation of the experimental data. For
example, if a first-order system is subjected to a step input, a semilog plot of the
data should result in a linear plot. Use of dimensionless parameters (e.g. Reynolds
number, Peclet number) may also provide important insights.
5. Correlate the data. The experimental data should be interpreted in terms of physical
theories or the basis of previous experimental work (done by others). The results
should be examined to see if they conform to or differ from previous
investigations or standards.

Sources of Errors
Errors occur in all experiments. Some of the errors can be avoided while others
cannot. Most of the errors that can be avoided are due to uncontrollable variables,
and/or lack of experience or carelessness on the part of the experimenter. These types
of errors can be avoided by carefully reviewing each step and condition (variable) in an
experiment and assessing whether they can significantly affect the outcome of the
experiment. If so, then the experimenter should alter the experiment, or pay particular
attention to certain aspects of the experiment, to ensure that a gross error does not
occur. As the saying goes, An ounce of prevention is worth a pound of cure. This

12

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A N A L Y S I S

B A S I C S

means that time spent preparing an experiment is well worth the effort. A great deal of
time and money can be wasted as the result of poor planning.
Beyond these controllable errors, there are errors of uncertainty. These are errors
that are beyond the control of the experimenter. There are two principal uncertainty
errors, fixed and random. Fixed, systematic, or bias errors are errors that are generated
repeatedly by the same amount for an unknown reason. For example, a ruler used to
measure length indicates a length of 1 m. However, the ruler actually measures 0.99 m
when compared to the actual standardized 1 m length. Thus, the ruler always measures
1 cm short per m measurement. These types of errors are often unknown. Calibration
of an instrument to an absolute standard, such as National Bureau of Standards (NBS)
standards, is the best way to detect and/or avoid systematic errors.
The second type of uncertainty errors is random errors. These errors are caused by a
variety of reasons that cannot be avoided such as experimentalist bias, fluctuations in
instrument readings, minor temporal variations in variables, etc. Every measurement
has a random uncertainty associated with it. This uncertainty is often related to the
accuracy of the instrument. For example, a pH probe may have an accuracy of 0.01
pH units within the pH range between 2 and 12. This means that, properly calibrated,
that this particular pH probe is accurate to within 0.01 pH unit between pH 2 and pH
12. Outside of those pH ranges, the pH probes accuracy may or may not fall within
that specification.

Uncertainty (Error) Analysis


Whenever a measurement is made there always is some uncertainty. The instrument
manufacturer may define this uncertainty, or may be estimated by the experimenter
(based on experience). Whatever the case, these measurement uncertainties are carried
on when a calculated result is generated. Many measurement uncertainties may be
associated with a single calculated result. The overall uncertainty for the calculated
result is a function of the error associated with each measurement. In general, this
overall uncertainty can be calculated as:
1

2
R 2 R 2
R 2
ET
e1
e2
en
x1 x 2
x n

where R = function of the independent (measured) variables, xi = independent


(measured) variable i, ei = uncertainty in measured variable i, and ET = overall
uncertainty in calculated function R.
As a simple example, consider the volume of a rectangular box that is determined by
measuring its dimensions with a ruler that has an accuracy of 0.2 cm. The measured

13

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B A S I C S

dimensions are L = 45 cm, W = 60 cm, and H = 20 cm.


measurements, volume would be 54,000 cm3.

Based on these

To determine the uncertainty of the volume:

V LWH
V
WH 6020 1,200cm 2
L
V
LH 4520 900cm 2
W
V
LW 6045 2,700cm 2
H
1

2
2
2 2

ET 1,200 cm 2 0.2 cm 900 cm 2 0.2 cm 2,700 cm 2 0.2 cm

620 cm 3

Statistical Analysis of Data


The purpose of this section is to not to provide a comprehensive overview of statistical
data analysis, but rather to review important concepts and outline appropriate
application of statistics to experimental data. Most of this information has been
covered in previous courses. More in depth coverage of statistical data analysis can be
obtained from course work or various textbooks.
Population Statistics
When a set of repeated measurements is made, the individual readings will vary from
each other. Most often statistical measures are used to describe the entire set of
measurements in terms of a centralized number, the spread of the data, and frequency
of distribution. Typical parameters include:
Arithmetic mean (or average) - x

1 n
xi
n i 1

Median - middle data point of a sequentially ordered data set. The datum for which half
of the data points in the set are higher and half are lower in value is the median.

14

D A T A

A N A L Y S I S

B A S I C S

Standard deviation - descriptor of the spread of the data compared to the mean =

n
2
xi x

i 1
n 1

12

Confidence interval - the probability that the actual mean value lies within a certain
number of values around an experimental mean. As an example, if a measured flow
reading has a mean of 100 and a standard deviation of 5, the 95% confidence interval
would be 100 1.96(5) = 100 9.8. In other words, there is a 95% probability that
the actual mean value is between 90.2 and 109.8.
Chauvenets criterion - sometimes one or two data points seem to be very different
compared to all of the other data points in a population. While it is logical to throw
out these types of data points, it is possible to apply a statistical test, Chauvenets
criterion, to determine whether data may be discarded. To apply this criterion, the
deviation of each data point from the mean must be calculated and divided by the
standard deviation: xi x / . The calculated value is compared to Chauvenets
criterion, which is a function of the number of readings in the population.
Number of
total readings
Max.
deviation,

10

15

25

50

100

1.38

1.54

1.65

1.73

1.80

1.96

2.13

2.33

2.57

2.81

xi x max /

Graphical Analysis
Experimental scientists and engineers are well known for the use of graphs to highlight
certain data trends and insights. However, random graphing of data usually generates
an excess of charts that are useless. Considerable thought must be given to the
physical phenomena involved in each experiment before preparing a plot. The person
who understands the physical processes (the theory) is usually the person who can
most successfully present experimental data graphically.
The most common graphical technique is the correlative graph in which the
relationship between two variables is plotted in a linear manner. To do this, the
experimenter must know what type of function will best describe the data. This
knowledge is based on theoretical understanding of physical phenomena.
A summary of plotting methods for various functions to obtain straight lines.

15

D A T A

A N A L Y S I S

Function
y ax b
y axb
y aebx

x
a bx

x
c
a bx

y aebx cs

Plotting Method
y vs. x on linear paper
log y vs. log x on log-log paper
log y vs. x on semilog paper
on linear paper

Slope
a
b
b log e
a

Y-intercept
b
log a
log a
b

y y1
x x1

vs. x on linear paper

b + cx1

x x1
y y1

vs. x on linear paper

b2
x1
a

a + bx1

1
y

y a bx cx2

B A S I C S

1
x

vs.

1 x x1

y
log
y1

c log e
vs. x on semilog

b + cx1 log e

paper
y 1 ebx

b
ya
x
yab x

log
1 y

vs. x on semilog

paper
y vs. 1/x on linear paper

y vs

on linear paper

The best method to determine the slope and y-intercepts for these various plots is the
use of the least squares method of linear regression, which is found in many standard
plotting software packages such as Excel.

16

L A B O R A T O R Y

E X E R C I S E S

Chapter

LABORATORY EXERCISES
This chapter contains summaries of the laboratory exercises that CHE and
ENVE 125 students will be conducting during this course.
As noted previously, there are a total of 10 different laboratory exercises for
CHE/ENVE 125. The four labs on basic laboratory measurement techniques and six
labs on instrumental analysis will be conducted over ten weeks.
The three laboratory measurement technique laboratories are:

Lab No.
1
2

Topic
Accurate volume measurement by using burets and pipet
Identification of a substance by acid-base titration

The five instrumental analysis laboratories are:


Lab No.
3
4
5
6

Topic
UV-Vis Spectroscopy: Determination of the cobalt and
nickel concentration
Atomic Absorption Spectroscopy (AAS)
High Performance Liquid Chromatography (HPLC)
Gas Chromatography (GC)

To reiterate there will be two students per lab group for laboratory measurement
technique experiments and four students per lab group for instrumental analysis
experiments.
Students are strongly encouraged to review the relevant sections in their texts prior to
conducting each laboratory exercise

17

E X P E R I M E N T S

Exercise # 1:
This lab period is designed to ensure precise and accurate use of basic laboratory
measurement techniques. These techniques will be needed throughout the rest of
the laboratory course and must be mastered to ensure the success of future
experiments.
1. Burets: Burets measure the volume of fluid delivered. The delivered
volume is calculated as the difference of the initial and final buret readings.
(It is noted that always starting from 0.00 on the buret may lead to a bias
error if the first graduation mark is miscalibrated.) Sources of error
include:
I.
II.
III.

IV.

Linear interpolation error in initial reading


Linear interpolation error in final reading
Limiting variations of the true volume due to nonuniformity in the bore of the buret, temperature
fluctuation during measurement, non-uniformity of
drainage
Determinate
error
(user
error):
Gross
reading/recording errors, bias (preference of even
digits, 0s or 5s)

a. Fill your buret with temperature-equilibrated deionized water.


Take an initial reading.
b. Deliver approximately 5 mL of water to a pre-tared container.
c. Record the buret reading. (Ensure that any excess water on the tip
of the buret is transferred to the weighing vessel by gently placing
the vessel to the tip of the buret.)
d. Record the final weight of the vessel.
e. Deliver approximately 7 mL additional water to the weighing
vessel.
f. Record the buret reading and new weight of the vessel.
g. Deliver approximately 10 mL additional water to the weighing
vessel.
h. Record the buret reading and new weight of the vessel.
Assuming the sample sizes are not too small, the relative standard
deviation of this experiment should be 1 to 2 %. You have used a
mass balance with much higher precision than the volume reading and
we will assume therefore that the weight measurement is exact based

18

E X P E R I M E N T S

on the number of significant figures in the reading. Therefore, you


should calculate the relative standard deviation by:
i.

Converting volume delivered by buret to mass delivered. (Consult


with your lab T.A. on the temperature of the water. The T.A. will
provide you with a water density chart based on water
temperature.)
ii. Calculating mass difference between buret measurement and
balance measurement for each delivered volume. (DM)

M1 2
M 2 2
M 3 2
) (
) (
) 1
W1
W2
W3
iii. RSD (

) 2 where W is the weight


3
3
3
determined by the mass balance.
If the RSD value is greater than 0.002 repeat the experiment. If you
fail again to achieve an RSD < 0.002, contact the TA for advice. If
your RSD is less than 0.002, have the T.A. initial that you have
completed this portion of the experiment.
(

2. Pipets. Pipetting is a valuable technique to deliver/transfer known


quantities of liquid. Pipetting is generally a more precise technique for
volumetric delivery than a buret if the volume to be delivered is known a
priori. Errors in pipetting include:
I.
Linear interpolation of initial reading (Note: pipets only have one
of these errors, burets have two)
II. Variability in drainage, temperature changes, and variations in
the size of the drop remaining in the pipet tip.
III. Gross user error.
It is important to always note the type of pipet used. The most common
type of pipet is the to deliver style. These are typically designated on the
pipet as td.
These pipets are designed to drain with gravity as the driving force and will
always have a small quantity of fluid left in the tip. Therefore, remaining
fluid should not be delivered using the pipet bulb.
a. Fill a pipet (5 or 10 mL) with temperature-equilibrated deionized water.
Deliver the fluid to a pre-tared vessel. Measure the final tare weight.
b. Repeat step a 2 times. (total of 3 measurements)
c. Repeat step a. This time use the pipet bulb to deliver all fluid in
the pipet. What is the error in delivering the full amount?
d. Calculate the relative standard deviation for your pipet work. The
RSD should be below 0.0015. If not, repeat experiment. If the
experiment still fails, contact your T.A.. Your T.A. will help you
determine the source of errors and correct them. Once you have

19

E X P E R I M E N T S

obtained a RSD below 0.0015, have your T.A. sign off on your
pipet abilities.
3. Put your above skills to use:
a. Prepare a 0.25 M aqueous solution of nickel(II) nitrate
hexahydrate, Ni(NO3) 6H2O. (MW = 290.81 g mol-1) using an
analytical balance, 50 mL volumetric flask (contains 50.0 mL at
calibration mark), and distilled water. Calculate the solution
concentration made to the appropriate number of significant
figures. (Note: you are aiming for approximately 0.25 M solution,
you tell me the exact concentration you made.)
b. Pipet 5 mL of your Ni2+ solution into a 50 mL volumetric flask
and dilute to 50 mL. (calibration mark is 50.00 mL; a 10 mL pipet
delivers 10.00 mL fluid)
c. Transfer the Ni2+ solution to a disposable cuvette. Measure the
visible light absorbance of the solution at 658 nm. Use distilled
water as a blank. Your T.A. will help you with this measurement.
4. Report: Your report need only consist of your T.A. signatures that you
completed the buret and pipet training, the concentration of your Ni2+
solution (with appropriate number of significant figures), and the
absorbance of your solution and blank.

20

E X P E R I M E N T S

Exercise #2: Determination of the concentration of KHP in


solution (Potassium Hydrogen Phthalate) in an unknown.
The unknown concentration of KHP in an aqueous solution will be determined
by titration with a standardized solution of NaOH. The equivalence point for the
titration will be determined using phenalphthalein as a color indicator. (Faintest
pink possibly perceptible).
During the first part of this experiment you will make 0.25 M NaOH and
standardize it against a primary KHP standard. The second part of the
experiment will use the standardized NaOH to determine the concentration of
KHP in the unknown sample.
You will be provided with pre-dried KHP of a stated purity. Keep the KHP in
the dessicator as much as possible to prevent the KHP from picking up moisture
from the laboratory air. Prior to coming to lab, determine the approximate

mass of KHP you will dissolve with 50 mL of water so that you will require
35-40 mL of 0.25 M NaOH to neutralize. Also be sure you know how to
calculate the amount of 6 M NaOH to dilute to obtain 500 mL of 0.25 M
NaOH.
1. Make 500 mL of approximately 0.25 M NaOH solution.

2. Accurately weigh out (record actual mass) your calculated amount of KHP and
dissolve into approximately 50 of de-ionized water. Use some of your dilution
water to help transfer any residual KHP in the weighing tray to solution. Also, be
sure to note the stated purity of the KHP for your later calculations. Add 1-2
drops of phenolphthalein to the KHP solution. Use your buret to accurately
deliver the NaOH until you have the faintest pink possibly perceptible. Be sure to
record the initial and final volume.
3. Repeat step 2 for a minimum of three total trials. (The greater the number of
trials, the more confident you can be about your measured concentration.)
4. Obtain from the TA your unknown KHP solution. Use a small portion of the
unknown for a sacrificial titration so you can estimate the volume of the
unknown necessary so that you use approximately 35-40 mL of NaOH when
titrating. Perform a minumum of three titrations to determine the molarity of the
unknown.
5. Report: The molarity of KHP determined for each trial, the average, and the
standard deviation.

21

E X P E R I M E N T S

Exercise # 3:

Determination of the Cobalt and Nickel


concentrations using spectrophotometry. (Adapted from
NJIT Chem 221 lab manual)
EDTA will be used to form a stable (colorful) complex with cobalt and nickel.
EDTA reacts with both of these metals at pH in excess of 4. You will make
calibration solutions for cobalt and nickel separately and determine their
absorption spectra. This will help identify the ideal wavelengths for measurement
of the cobalt/nickel mixture. Using beers law and a linear combination of
equations you may determine the concentration of both components in the
unknown solution.
Procedure:
1. Pipet duplicate 40 mL aliquots of Ni and Co standard samples into four
100 mL volumetric flasks. Add 10 mL of buffer (1 M NH4Cl, 1 M NH3 in
water, prepared in advance by your T.A.) to each flask. Add 1.6 g
disodium salt EDTA. Stopper and warm flasks on a hot plate for 20
minutes to ensure complete formation of the complex. Cool and dilute to
volume. Prepare a blank containing 12 mL buffer solution, 1.6 g disodium
EDTA in 100 mL of solution.
2. Use the spectrophotometer to scan the absorbance of each solution
between 350 to 650 nm. From the curves, determine the optimal
wavelengths to measure cobalt and nickel at.
3. Pipet duplicate 40 mL aliquots of the unknown solution into two 100 mL
volumetric flasks. Add 3.8 g EDTA and 10 mL buffer, warm for 20
minutes, and measure the absorbance of each of the standards at the two
wavelengths determined in step 2. Make at least five readings at each of
the wavelengths.
4. Report: Concentration of cobalt and nickel in the unknown solution
determined for the duplicate unknowns.

22

E X P E R I M E N T S

Exercise # 4: Atomic Absorption Spectroscopy


Atomic Absorption Spectroscopy (adapted from NJIT lab manual)
Flame atomic absorption spectroscopy is widely used for analysis of most
metals because of its simplicity, effectiveness, and relatively low cost. In this
lab we will use flame AAS to determine the sodium content in an unknown
solution, and in some snack foods. Sodiums characteristic wavelength for AA
analysis is 589 nm.
Procedure:
1. Make 200 mL of dilute nitric acid (HNO3) by a 1:1 dilution of
concentrated HNO3. Prepare 5, 10, 15, and 20 ppm Na standard solutions
by diluting your stock solution (concentration given on bottle) with
deionized water. You dilute nitric acid will serve as your blank.
2. Unknown. Obtain your unknown from your lab T.A. The T.A. will
instruct you on how to use the instrument. First, measure the absorbance
of the blank, then the standards starting from lowest to highest
concentration. Measure the absorbance of the blank again before
measuring your sample.
3. Snack food determination. You need to bring some snack food for this
lab. Make sure you look at the snack food label. First you must get
the snack food into the appropriate form for analysis. Grind and mix
some of the snack food you have brought. Weigh out triplicate 0.50 g
samples into 200 mL Erlenmeyer flasks. Add ~50 mL of dilute HNO3.
Place on hot plate in fume hood and bring to a boil. Simmer for 30
minutes. Cool and transfer (quantitatively) your solution to a 100 mL
volumetric flask. Dilute to the mark with distilled water and mix
thoroughly. Filter each solution through filter paper into a clean, dry 100
mL flask. Measure using the AAS. If the value is out of range (high),
dilute and repeat. You should do this for three separate snack foods of
your choice.
4. Report: Sodium in unknown sample (ppm). For the snack food report the
sodium as a percentage of the food. Be sure to compare to value on
package.

23

E X P E R I M E N T S

Exercise # 5: High Performance Liquid Chromatography


An HPLC analysis of the artificial sweetener, aspartame, in beverages.

SCOPE AND APPLICATION


This analytical procedure is for the identification and quantification of aspartame
present in an artificially sweetened beverage.

SUMMARY OF METHOD
For this lab, you will use an Agilent high performance liquid chromatograph (HPLC)
equipped with a DAD detector to identify and quantify the concentration of
aspartame. You will use a calibration standard to identify the retention time of
aspartame and generate a calibration curve.
The HPLC sample injection, column, and operating conditions will be set up prior
to the lab. We will use a 10mM Potassium phosphate dibasic (pH 6.3, adjusted
with phosphoric acid) mobile phase buffered at a flow rate of 1.0ml/min. The
detector wavelength will be set to a single channel at 210 nm.

EQUIPMENT AND SUPPLIES


Agilent 1200 HPLC system:
Vacuum Degasser
Quatenary Pump
Standard Autosampler
Diode Array Detector
Agilent Chemstation Software
Agilent ZORBAX SB-C18, 5 um, 150 mm 4.6 mm
Agilent LC Setup per SAE 930142
Required Chemicals:
Water (HPLC grade)
Potassium Phosphate Dibasic (HPLC grade)
Phosphoric Acid (HPLC grade)

Procedure:
1. You will be provided with pure aspartame to generate your calibration
solutions and determine the retention time of aspartame. Using serial
dilutions, you will make 5 solutions in a range of concentrations for your
calibration curve. You should have an idea of what range to calibrate for.
You will use methanol as your solvent. Inject these into the HPLC.

24

E X P E R I M E N T S

2. Using the HPLC software, integrate the each chromatogram to determine


the peak areas of aspartame at each concentration. Generate a calibration
curve with this data.
3. You will need to bring in an artificially sweetened beverage that

contains aspartame (Nutrasweet).

4. Bring the beverage to room temperature. If the beverage is carbonated, it


will need to be degassed by letting it stand out for a few hours. Filter
~10ml of the beverage into a clean labeled vial. Transfer ~2ml of this
volume to autosampler vials.
5. Inject the sample into the HPLC.
6. Using the HPLC software, integrate the chromatogram to determine peak
area of aspartame and quantify it using your calibration curve.

25

E X P E R I M E N T S

Exercise # 6: Gas Chromatography


You will use the gas chromatograph (GC) to identify and quantify the
concentrations of three organic compounds. In this lab you will be given a smallcapped vial of the unknown and a choice of four possible organic compounds.
Based on the retention time index of each compound you should be able to
identify the unknown species. You will then produce a calibration standard to
identify the concentration of the unknown species.
Procedure:
7. The possible organic compounds in your unknown are cyclohexane,
benzene, toluene, and heptane. Note: The GC has an auto-injector that
will inject 1 mL of a given compound into the system. You will use
methylene chloride as your solvent. The unknown mixture concentrations
are in the range of 50 ug/mL to 250 ug/ml.
8. Before coming to lab, develop a strategy to identify your

compounds.

9. The TA will show you how to use the instrument, the separation column
used, and the temperature program that will separate these compounds.
10. Prepare calibration standards for the compounds identified. This is done
by serial dilution of the stock hydrocarbons. If you semi-quantitatively
performed step 2, you should have an idea what range to calibrate for. A
minimum of three points is necessary for a good GC calibration.
11. Report: identity of unknowns and their concentrations.

26

E X P E R I M E N T S

Chapter

GUIDELINES FOR LAB REPORT


PREPARATION AND GRADING
CRITERIA
This chapter contains the guidelines for Lab report submission of the laboratory
exercises that CHE and ENVE 125 students will be conducting during this
course.
General Rules:
- The group grade for all lab reports will be worth 50 points. The point break down
for each section is as follows:
o Front Matter: 2 points
o Introduction/Background: 10 points
o Experimental Apparatus and Procedures: 10 points
o Results and Discussion: 15 points
o Conclusion: 6 points
o References and Appendices: 2 points
o Xerox Copies of Laboratory Notebook: 5 points
-

All reports must be prepared using a word processing system such as Microsoft Word or
comparable. Figures should be prepared using Excel or similar. Tables should be
prepared using Microsoft word as well. HANDWRITTEN WORK SHOULD NOT
BE GRADED.

An individual grade for each member of the group will also be assigned based upon the
quality of their contribution to the report. This grade will also be out of 50 and the
average of the individual and group grade will represent the students overall grade for the
lab report [Average of the individual = 50% individual grade + 50% of the group
grade]. If more than one-person works on a section, both will receive the same individual
grade for that section. This total out of 50 should be determined from the sum of the
points earned by each member on their respective sections.

ALL writing should be in complete sentences with appropriate grammar and spelling.

27

E X P E R I M E N T S

Writing should be in the third person and the past verb tense should be used.

Writing should be specific and concise (not rambling, redundant and repetitive).

There should be no blank or free space anywhere in the report.

All equations should be numbered.

In total, the reports for experiments in which an experimental protocol was provided
should be no more than 10 pages of written text. Note these page limits are not a requirement.
In total, the written portion (Intro, Experimental, Results and Discussion, Conclusions,
and References) should not exceed these limits. The front matter (Title, Table of
Contents, List of Table and Figures) does not count toward this total, nor do Figures and
Appendices.

Pages should be numbered. Additional details: the cover should not have a page number;
the table of contents and list of tables and figures should be pages i and ii, respectively;
the first page of your report is 1 and all subsequent pages are number in the appropriate
progression.

Section Grading Criteria:

1.

Front Matter (2 points):

Does the report include a:


- Cover page that identifies the experiment number and title, the due date of the
report, and the group number and group members.
- A table of contents that lists all the section headers and the page in the report
where that section is located. The table of contents should also indicate which
member of the group contributed to each section.
- A list of tables/figures including the appropriate table/figure number, table/figure
title, and the page in the report where the table/figure can be found.

Are these items located at the front of the report (the first 3 pages; note, these do not
count against your page total).

2.

Introduction and Background (10 points):


-

Generally, the introduction should provide:

o a clear statement of the goal and objectives for the experiment


o background information that is needed to understand the remainder of
the report.

o additional references to pertinent literature related to the project.


-

3.

All equations and topics that are not common knowledge should have references.

Experimental Apparatus and Procedures (10 points):

28

E X P E R I M E N T S

4.

5.

6.

This section should provide sufficient information on the apparatus and


experimental procedures.

It should be written in the PAST TENSE (e.g., we measured not we measure

It should not be a copy and paste of the laboratory manual. Without a reference,
this is plagiarism.

Results and Discussion 15 points):


-

This section should give the results of the experiments in tabular and/or graphical
form. Each table and figure should be numbered (e.g., Figure 1 or Table 1) in the
appropriate order discussed in the text.

In addition, a brief narrative discussion of EACH table and/or graph should be


given. Discussion should focus on important features of the data and not be simply
a repetition of numbers.

All tables and figures should be located at the end of the written portion of the
report (after references but prior to the appendix). Be sure they:
o Present clear and informative figures and tables. Make sure all variables are
defined. For figures, make sure all axes are labeled (with units), that they use
legends to distinguish between multiple sets of data, and avoid the use of colors
unless they print the document in color.
o Put the tables before the figures at the end of the report.
o Number each figure and table according to the order they are discussed in the
text.
o Provide each figure and table with a title and caption. Both the title and caption
should be in sentence form and be as descriptive (yet concise) as possible.
Captions should not be used to discuss or interpret the figure. Rather, it should
clearly describe what the figure/table presents, and in the case of figures with
data, list key conditions under which the data was collected.
o Be sure that all figures and tables are discussed in the text.
o Figures are visually appealing (no border, minimal gridlines, do not overlap
regression lines with lines connecting data points)
o Make sure appropriate significant figures are used in all calculations and in
reporting all values.

Conclusion (6 points):
-

This section should summarize all important results and interpretations in light of
goal and objectives for the experiment.

At least one recommendation should be made for further study or improvement in


the experiment. If no recommendations are provided, a justification for the omission
must be stated.

References (and Appendices): 2 points


-

A list references used in preparing the report must be provided

Appropriate bibliography formatting must be used. For example, if citations in the


text are by number, this list should correspond to the numbering system. If (Author,
Year) notation is used for citations, the list must be alphabetical.

29

E X P E R I M E N T S

7.

Wikipedia and similar web pages are NOT acceptable sources for scientific literature.

The appendices should include all additional information relevant to the experiment
but not necessarily integral to the experimental write-up. Specifically, raw data tables,
raw data collected from analytical instruments, example calculations, etc. should be
included here.

The appendix should be located after table and figures

Xerox Copies of Laboratory Notebook


-

Each student in the group must attach Xerox copies of his/her laboratory notebook
pages that are relevant to the particular lab after the Appendix.

These pages will be graded out of 5 points

30

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