Forward

Your laboratory work is the core of your chemistry course. Laboratory work will be based on how you conduct yourself in the lab. This
include how you practice safety, carry out experimental protocols, make observations and how you document your while observations in your
lab notebook. You will be graded on how you handle equipment and instruments. How you communicate your findings will culminate the
mastery of each module covered in this course. You have a challenging opportunity to observe many of the facets of chemistry under
controlled laboratory conditions and to experience first-hand the method of inquiry that is the foundation of all experimental sciences. The
chemistry laboratory illustrates the scientific method in action. Here are a few brief points that will give you a good start in this course.

1. Gain self-confidence by working individually, unless the experiments require teamwork. Don't hesitate to ask questions if you are
uncertain about a procedure, the interpretation of results, or the calculations.

2. Use your ingenuity and common sense. Laboratory directions, while quite specific, leave ample opportunity for clear-cut, logical,
original, and imaginative thinking. This attitude is a prerequisite in any scientific endeavor.

3. Don't waste time by coming unprepared to the laboratory. Prepare for each experiment by studying all aspects of the experiment.
Review lab procedures and/or theories from other sources if you are uncertain about certain aspects of the lab.

4. Prepare your “Laboratory Reports” for each experiment with care. To record your data, use a permanently bound notebook as
prescribed by your instructor. All data should be recorded directly into your laboratory notebook, not on loose sheets or scraps of
paper. If calculations are involved, show an orderly calculation for the first set of data, but do not clutter the calculation section
with arithmetic details. Likewise, think through and answer important questions that are intended to give you an understanding of
the principles on which the experimental procedure is based as you perform the experiment.

5. Scientists learn much by talking with one another. You may learn a lot by talking to your classmates, but not by copying from them.
Integrity is the keystone of scientific work. You will also profit by referring to your text while working in the laboratory. (Books
are generally an even more reliable and complete sources of information than are your classmates!)

6. For tabular data on the properties of substances, you may wish to consult handbooks such as the Handbook of Chemistry and
Physics (CRC Press, Inc., Boca Raton, Florida) or Lange's Handbook of Chemistry (McGraw-Hill, New York).

SAFETY RULES
Familiarize yourself with the safety rules given in the lab manual. Observance of these rules, as modified or added to by your instructor, is
essential for the sake of your safety and that of others in the laboratory. Your instructor will indicate the location and show you the proper
use of the fire extinguishers, fire blanket, eyewash fountain, safety shower, and first-aid cabinet and supplies. The instructor will also tell
you when you should wear safety goggles.

GOOD LABORATORY PRACTICES

Familiarize yourself with the good laboratory practices in the lab manual. It is essential that these regulations, as modified or added to by
your instructor, be followed carefully and to the letter.

BASIC LABORATORY EQUIPMENT AND PROCEDURES

Check the equipment in the laboratory locker assigned to you as directed by your instructor. Before your first laboratory experiment, read
over the introductory part on common lab techniques i.e., handling of chemicals, care of laboratory glassware, and volumetric measurements
of liquids, etc.

Supplemental information can be found in the following website:

http://faculty.sdmiramar.edu/fgarces/zCourse/All_Year/Ch251/bFrames/Content_Frames_AChem.htm
http://www.youtube.com/subscription_center?add_user=fgarcesch251
http://faculty.sdmiramar.edu/fgarces/LabMatters/Instrument.htm
http://faculty.sdmiramar.edu/fgarces/Links_Lib/Link.htm
http://faculty.sdmiramar.edu/fgarces/ChemComon/Testphobia.htm
http://faculty.sdmiramar.edu/fgarces/ChemComon/Tutorial/Tutorial.htm

J.L.Roberts, J.L.Hollenberg, J.M.Postma "Chemistry in the Laboratory" 4th Ed., Freeman. 1997
ii
 Miramar Chem. Laboratory Policy and Procedure 8/18 -FG

Welcome to Miramar College's Chemistry 251 laboratory. This is Quantitative Analytical Chemistry or specifically, qualitative and
quantitative analysis of chemical systems. We have a number of policies that should always be kept in followed when working in the
laboratory. Outlined here are policies that will be strictly enforce so that your safety is never compromised. Remember to follow Good Lab
Practice (GLP) at all times. Please be sure read everything carefully and follow the policies that must be followed when you arrive the
laboratory, S6-203.

1. All students are required to have, and wear, safety goggles when conducting experiments (Googles not glasses). From this point on these
safety equipment will be referred to as Personal Protective Equipment (PPE). You must adhere to the safety rules outline for this course,
there are NO exceptions to this rule. Goggles must always be over your eyes when lab begins. These are available for purchase at the
bookstore. If you are not wearing your goggles, do not proceed with the experiments. Your instructor will not allow you to be present in the
lab classroom. You should bring safety goggles by the time you begin with the first experiment. Some instructors will penalize your lab
safety quiz up to 50% off for not bringing or using your goggles during experiments.

2. All students are required to wear safety gloves (nitrile not latex since some students are allergic to latex) when conducting experiments.
Remove gloves when leaving the classroom. The idea is not to cross-contaminate areas that has not been exposed to chemicals. Remove
gloves and dispose of in the proper solid waste refuse.

3. All students are to wear proper attire when present in lab. That means clothing that minimize skin exposure. Furthermore, students are
to wear cotton lab coats (white) when conducting lab work at all times. When leaving the lab (for bathroom or lunch break) remove lab coats
and leave in your equipment drawer. Upon returning to continue lab work, put back on your lab coat.

4. Each student must purchase a Master™ Combination lock with the following serial numbers: V99XXX, V629XXX, or 10976xxx (the last
three numbers are different from lock to lock). These special Master™ locks can be opened by the lab technicians with a master key. The
Miramar Bookstore sells these locks, and it is departmental policy that all students must exchange the department's brass locks with these
Master™ combination locks by the second week of the term. If you do not have a lock, the instructor will ask you to go to the bookstore to
purchase these locks before being allowed to perform an experiment. All other locks that do not conform to the Master™ Combination lock
just described will be cut off. Lab techs must have access to student lockers at all times in case of emergency.

5. Students will be allowed into class no earlier than ten minutes prior to the start of class and they are not allowed in the lab at any time
without an instructor present. Please do not disturb the instructional lab techs from completing their jobs.

6. The department has a very strong HAZMAT policy. Absolutely no chemicals—not even things like Sodium Chloride and Sucrose are
allowed down the sinks. Contamination of the drain by toxic chemicals cannot be compromise. The department has a blanket policy that all
chemicals must be disposed of in the proper waste container. Violation of this rule will result in a grade adjustment on the student’s lab
reports because of poor lab practice.

7. The MSDS library is accessible for all students and is kept in the tech prep area. You can also access this information by going to:
www.reade.com/MSDS_Links.html or chemfinder.com. Also available in the lab, are the Merck handbook and the Handbook of Chemistry and
Physics. The reference texts are for student use. After using these reference texts, students should return them back to the instructor
desk.

8. Students are not allowed in the chemical storage room or the prep area for any reason. You will be allowed to use the instrument room
but please do not enter the prep area or the chemical storage room. These rooms are to the left of the balance room.

9. Equipment such as hot plates, ring stand and other hardware are found in various locations around the lab. Cabinets housing equipment will
be properly labeled. Certain equipment such as Vernier probes or burets will be on a cart at the rear of the room. Students must return all
equipment clean and in working condition back to its proper area before leaving the classroom. Under no circumstances are community
equipment (i.e., hot plates) to be kept in student lockers or in the workbench.

10. Students are not allowed to keep other supplies that has been set out for each experiment such as: Vernier probe, laptop computers,
stop watch and so on in their lockers. Violating this rule will result in poor lab grade.

11. Students are not allowed to use the phones in the classroom under any circumstance. Please turn off your cell phone upon entering the lab.
Usage of cell phone will reflect lab technique scores.

12. It is the responsibility of the students of each lab to clean the laboratory before leaving. The lab techs work very hard to keep clean
and uncluttered. All students should clean messy lab benches and sink areas, push in their chairs before leaving the classroom; each student
is responsible for picking up after themselves. The difficulty of the pop quizzes and midterm assessments have a direct correlation to the
state by which the lab is kept during the semester.

Please, if you have any questions do not hesitate to contact the lab tech or the instructor. The chemistry lab techs for this course is Afshin
Nour (619) 388-7438. The other lab techs are Dam Le (388-7437), Tien Nguyen (388-7390) and Aleena Vargas (388-7826

iii
Lecture Course Outline: Lab Course Outline:

Tools of Analytical Chemistry Safety and the Lab Notebook

Measurements Calibration of Volumetric Glassware
Tools of the Trade Preparation of Solution and Standardization
Experimental Errors
Classic Method of Chemical Analysis
Statistics
Gravimetric Analysis
Quality Assurance and Calibration Analysis unknown metal by precipitation of sulfates
Sintered-Glass Filtration
Ashless Filter Paper Procedure
Chemical Equilibria
Titration Fundamentals Titrimetry Analysis
EDTA Titration of Metal Ions
Chemical Equilibrium
Iodometric Titration of Vitamin-C
Activity and Systematic Treatment of Equilibrium
Quantitatively Determining the Acid Content in Fruit
Monoprotic Acid-Base Juice
Polyprotic Acid-Base Evaluating Commercial Antacids
EDTA Titration Determination the content of Vitamin-C due to
Advance Topic in Equilibrium effects of cooking.
Manganese analysis by EDTA titration

Electrochemical Analysis
Electrochemical Methods
Electro gravimetric Analysis of Copper
Fundamentals to Electrochemistry Measuring Vitamin C in Fruit Juice by Voltammetry
Electrodes and Potentiometry Polarographic Measurements of an Equilibrium
Redox Titration Constant
Electroanalytical Techniques Ionization constant of weak acid by potentiometric
Titration

Spectrophotometric Analysis
Spectrochemical Methods Spectrophotometric Determination of Copper in Brass
Application of Spectrophotometry Spectrophotometric Determination of Iron in Vitamin
Spectrophotometers Tablets
Atomic Spectroscopy Spectrophotometric Analysis of Caffeine & Benzoic
Mass Spectroscopy Acid in Sodas
Spectrophotometric Analysis of manganese in steel
Special Topics: IR and NMR
Fluorometric Analysis of Vitamin Tablets for
Riboflavin
Spectrophotometric analysis of Co(en)22+ isomers
Separation Methods Determination of sodium in Soda Pop
Intro to Analytical Separation
Gas Chromatography Separation Methods
Thin-Layer Chromatography Paper Chromatography Separation and Identification
of Metal Ions Preparation and analysis of Ferrocene
High-Performance Liquid Chromatography
Measurement of carbon monoxide by GC
Chromatographic Methods & Cap. Electrophoresis
Analysis of Analgesic Tablets by HPLC and IR
HPLC determination of Caffeine and Sodium Benzoate
in Soda
Gasoline component by GC / LCMS
Ethanol in mouth wash by GC / LCMS
Qualitative and Quantitative, HPLC Analysis of Vit-C
in Fruit Juices

iv
 Lab Manual Chemistry 251 L Page #

Forward i
Miramar Lab Policy and Procedure ii
Lecture and Lab Course Outline iii
Table of Content iv
INTRODUCTION 1
Typical Laboratory Equipment 3
Laboratory Locker and Inventory 4
General Writing in the Science Lab 4
I Resources and Style 4
II Keeping up with the Laboratory Notebook 6
Notebook Pages Example 7
III The Lab Notebook Content 8
ACS (American Chemical Society) Style Guidelines Quick Guide 9
IV Grading Rubric for Lab Notebook and Post-Experiment Write-up 11
Experiment Lab Notebook Write-up Criteria 14
Statistical Treatment of Experimental Measurements 15
Laboratory Safety Contract 19
Safety Quiz 20
ACTIVITIES 21
A-1 Review of Basics 23
A-2 Penny Statistics 25
A-3 Chemical Equilibrium and Acid-Base 29
A-4 Electrochemistry Basics 33
A-5 Spectroscopy 37
A-6 Chromatography 43

EXPERIMENTS 47
E-00 Basic Laboratory Techniques, Compliance of GLP and Calibration of Glassware 49
E-1 Molar Mass of an Unknown Sulfate Salt by Gravimetric Techniques 65
E-2 EDTA Titration of Ba2+ of a) Unknown metal sulfate and b) Unknown BaCl2 73
E-3 Iodometric Titration of Ascorbic Acid 81
E-4 Quantitative Analysis of Ascorbic Acid Using Cyclic Voltammetry 87
E-5
E-7
E-8
APPENDIX
Practical
Apx-1 Caring and Handling of Chemicals
Apx-2 Measurement of Mass
Apx-3 Measurement of Volume
Apx-4 Titration Technique
Apx-5 Using the CARY UV-VIS Spectrometer
Apx-6 Electromagnetic Spectrum
Apx-7 Physical Properties of Water: Density and Vapor Pressure of Water
Apx-8 Acid-Base Indicators / Common Laboratory Acid/Base Solutions
Apx-9 Acid Dissociation Constants
Apx-10 Standard Reduction Potentials
Apx-11 Thermodynamic Quantities for Selected Substances
Apx-12 Logger Pro 3, Quick Reference
Apx-13 Miscellaneous Chemical Information and Equations
1
 INTRODUCTION

INTRODUCTION

INTRODUCTION

INTRODUCTION

1
2
Typical Laboratory Equipment

3
Chem-251 Laboratory Locker Inventory
Name:_______________________________________ CSID ___________________________Locker #____

Rec' Ret' Article Rec' Ret' Article

3 ribbed watch glass 4 cork rings
3 watch glass 1 volumetric flask, 100 mL
3 crucibles, porcelain, with cover 2 volumetric flasks, 250 mL
1 Walter crucible holder 1 volumetric flask, 500 mL
2 buret caps 1 volumetric pipet, 10 mL
3 crucibles, porous, filtering 1 volumetric pipet, 25 mL
1 pair crucible tongs 1 pipet bulb
1 graduated cylinder, 10 mL 3 beakers, 1000 mL
1 graduated cylinder, 25 mL ground glass stopper
1 graduated cylinder, 100 mL 3 beakers, 600 mL
3 funnels, 3" long stem 3 beakers, 400 mL
1 funnel, short stem 3 beakers, 250 mL
2 medicine droppers 2 beakers, 150 mL
3 Clay triangles 3 beakers, 100 mL
3 rubber policemen 2 beakers, 50 mL
3 stirring rods 3 bottles, plastic, 1 L
3 watch glasses, 5" or 6" 1 desiccator, lid, and support
3 watch glasses, 4" or 4 1/2" 1 filtration flask, 500 mL
3 watch glasses, 3" or 3 1/2" 4 Erlenmeyer flasks, 500 mL
1 watch glass, 2 1/2" 7 Erlenmeyer flasks and/or
Phillips beakers, 250 mL
3 watch glass supports 1 Erlenmeyer flask, 50 mL, with
1 wash bottle, plastic, 500 mL 1 spatula
1 wash bottle, plastic, 250 mL 1 scoopula
6 weighing bottles, with lids 1 buret, 50 mL SN#
1 buret, 25 mL SN#

4
 General Writing in the Chemistry Lab

I. Resources and Style- Scientific writing is not limited to scientific journal articles. Scientists on every level are more likely to achieve
success if they are able to describe their work and explain its significance to others. Technical writing can vary from a brief explanation
of how to use a piece of equipment to a lengthy report on the activities in the laboratory. Technical writers produce articles written for
the layman explaining technical subjects in understandable terms. Effective technical writing is a job skill that is very much in demand.
College-level assignments that involve report writing on technical subjects require the same considerations as professional writing.
First, consider the audience. Will a skilled professional or a layman read the material? In this case it will be your instructor, (consider
him/her a skilled professional) but never assume however that your instructor is familiar with the basic principles of the field being covered;
you must include some basic background information, with special attention given to explaining technical vocabulary that is specific for the
topic being discussed.
Most writing projects begin with a visit to the library or the internet to find appropriate background materials. Again, the level of the
project will determine how the information search is conducted. Other information contained in scientific journals can be found through
indexes such as those provided in Chemical Abstracts; using the abstract indexes is a skill that must be developed through practice. Many
science reports, however, require only limited keyword search using Google Scholar. Some useful links as sources of background information
include:

General Chemistry Resources Links for scientific writing:

http://www.chem1.com/acad/webtext/virtualtextbook.html http://www.lib.berkeley.edu/CHEM/acsstyle.html
http://en.wikibooks.org/wiki/General_Chemistry http://www.monroecc.edu/depts/library/acs.htm
http://en.wikipedia.org/wiki/Chemical_Science_%28journal%29 http://en.wikipedia.org/wiki/Technical_writing
http://pubs.acs.org/journal/jceda8 http://en.wikipedia.org/wiki/Scientific_writing

Dictionaries can be useful in defining technical terms or concepts. Those useful in chemistry include:
Chamber's Dictionary of Science and Technology (McGraw-Hill)
Chemist's Dictionary (Van Nostrand)
Hanckh's Chemical Dictionary (McGraw-Hill)
McGraw-Hill Dictionary of Scientific and Technical Terms

Facts and data are found through many scientific handbooks. Some used in chemistry papers include:
CRC Handbook of Chemistry and Physics
CRC Handbook of Environmental Control
Merck index

Review articles in periodicals like Scientific American, Science, and Nature give useful information on a variety of scientific topics.
They can be conveniently found through the General Science Index, which provides a comprehensive subject index to English language
periodical literature in the sciences. A major resource of the library not to be neglected is the expertise of a good science librarian.
Technical writing depends no less than any other form of writing on the basic language skills of the writer. Incorrect spelling and
grammar can mar the effect of the most interesting and original narrative. A good guide to English usage belongs next to a dictionary on
the writer's desk. Good writing style is developed through practice in writing and rewriting. A clear, direct style contains no unnecessary
words. For example, consider the following example:
At this point in the experiment the mixture was heated up through the use of a hot plate.
An improved version is:
The mixture was heated with a hot plate.
Some science publications prefer the use of the first person ("I heated the mixture") be avoided. Use of the passive voice "the
mixture was heated" is then indicated. In other uses the more direct form of the active voice may be preferred, as in, "We decided to
heat the mixture" rather than, "It was decided that the mixture should be heated." When writing instructions, the imperative is often a
good choice: "Heat the mixture on a hot plate" is more direct than "The mixture should be heated on a hot plate."

There are many references available to help you develop the valuable skill of communicating information.

General references include:

W. Strunk, Jr.; E. B. Write. The Elements of Style, Macmillan: New York, 1979.
Margaret Shertzer. The Elements of Grammar, Macmillan:: New York, 1986.

References pertaining to technical information are:

B.Edward Cain. The Basics of Technical Communicating; American Chemical Society: Washington, DC, 1988.
Anne Eisenbero. Writing Well for the Technical Professions; Harper and Row: New York, 1989.

5
II. Keeping up with the Laboratory Notebook:

"A laboratory notebook is one of a scientist’s most valuable tools. It contains the permanent written record of the researcher’s
mental and physical activities for experiment and observation, to the ultimate understanding of physical phenomena. The act of
writing in the notebook causes the scientist to stop and think about what is being done in the laboratory. It is in this way an
essential part of doing good science." “The foremost reason for using a bound notebook rather than a loose-leaf binder or spiral
notebook is that the pages are permanently and strongly attached together. The date of a particular entry is less subject to
question if notes are recorded in a chronological order with no blank or missing parts. The industrial researcher, whose work may
lead to patents, has no choice except to use a bound notebook for all laboratory note taking."

From Writing the Laboratory Notebook by Howard M. Kanare; American Chemical Society 1985
The scientific notebook is the scientist's own record of experiments performed and phenomena observed. Beginning with the first student
laboratory report there are special requirements for recording experimental results. The requirements may seem rigid at first, but they
are very understandable in light of the purposes of the notebook.

For the professional scientist the claim to original work is found in the scientific notebook. Millions of dollars in patent rights may
depend on the existence of a properly dated and authenticated scientific notebook. Many of the rules that are followed in recording data
follow from this important function of the notebook. Nothing is ever erased; and incorrect reading is crossed out and the correct one
written beside it. Work is recorded in a bound notebook with pages that cannot be removed or added. Every entry is dated, signed, and
countersigned by the scientist in charge of the laboratory. All these rules are designed to produce a record that will constitute proof not
only of what experiments were performed, but of the exact date. This is important, because if two scientists make the same discovery,
the first one to do so will gain all the legal rights and most of the credit for the work. Obviously, it is more important to have a complete
and original record than a perfectly neat one. A few crossed-out readings are not uncommon, and a few blots from spilled chemicals are
not unheard of either. These are preferable in the laboratory notebook to a perfect page that has been copied over at a later date and no
longer constitutes an authentic original record. Under no circumstances is data to be recorded on loose paper rather than directly into
the notebook! If you write your data or observations on loose pieces of paper, at best you lose 5pts or up to 20% per violation and at most
you will receive zero for that day's lab technique grade.

Another important function of the notebook is to record the procedure and observations so clearly and completely that the experiment
can easily be repeated at a later date. Experiments that cannot be repeated by the same researcher or by other laboratories are soon
discredited. For the student in the laboratory, complete notes are important as well. If something goes wrong, it should be possible to find
the error in procedure from the lab notebook. At times, the numbers in the crossed-out data entries tell an interesting story. Occasionally
an interesting and unexpected phenomenon will be observed that merits further study. Keeping a complete clear record of what has
happened in the laboratory is essential.

In order to keep a complete record, each experiment entered into the notebook should include certain features. On each page entry, the
scientist's name and the date should be entered. The title of the experiment being performed is an important element that is often
neglected. "Chemistry Lab" is an inadequate substitute for the experiment title, which is usually readily available. Often it is useful to begin
by writing the objective, or the purpose, of the experiment. Stating the objective clearly helps both the experimenter and the reader of
the notebook to understand the experiment. A complete record of experimental procedure is essential, either as a step-by-step description
or a pictorial flowchart followed by a complete reference to a standard experimental procedure. If a standard procedure is given, great
care must be made to note any deviations from that procedure. A list of materials and equipment used can be a great help in organization
if it is included as a part of the experimental procedure. Finally, a description of any safety or hazardous guidelines should be included.

Though the laboratory notebook does not have to be perfectly pristine, it is certainly desirable that it should be as organized as possible.
Some time and thought spent in planning before the laboratory period begins will result in a better notebook and a more successful
experiment. As mentioned above, the date, title, experimenter's name and objective of the experiment should be entered before the
experiment begins. If the experimental procedure that has been provided does not already give labeled data tables for an experiment, it
is worth some time and thought to set up such tables before entering the laboratory, rather than waste time during the experiment deciding
how to do so. Ample space should be provided not only for the expected data, but also for corrections and notes. Unused space can be
crossed out later as necessary, though extra pages are never torn out. Sometimes only the right-hand pages of the notebook are used,
leaving the other pages free for later notes or calculations. Individual research laboratories or student laboratories may have standard
notebooks or forms in which to write laboratory results. All of them share the basic objective of recording in a useful way the scientist's
actions, observations, and thoughts while in the laboratory.

6
Notebook Pages Examples
The following illustrate the proper manner in which a laboratory notebook should be kept. These pages are reproductions of a student's
general laboratory notebook. The style of this notebook conforms to the guidelines presented in next section of this manual.

Before entering the laboratory, the student had written the complete heading on each page and the objective of the experiment. This is
followed by some background information and a pictorial flowchart. A sample data table was sketched and the safety precautions were
written.

In another experiment a student writes up the section of data/results with detailed observations of what happened during the experiment.
The second example below shows a student performing several calculations based on the data collected with the step by step calculations.

7
III. The Lab Notebook Content

When the scientist prepares a formal written report of experiments performed in the laboratory, the report follows a generally
accepted outline. Introduction, results and discussion/conclusions follow in order as separate sections and these are clearly labeled. Lists
of references and even the title are treated in standard ways. All this is typed in a journal type format.

The Title of a scientific paper is seldom an occasion for creativity. Titles for articles in scientific journals are carefully constructed
from words that will be useful key words for information searches by computer. Titles for student laboratory reports are usually indicated
in the assignment. As with the laboratory notebook, "Chemistry Laboratory" is unacceptably vague as a laboratory report title.
Abbreviations as part of a title should be avoided.

The Introduction section should make clear to the reader the purpose and the background of the experiment. The objective of the
work that is being discussed should always be clearly stated. It may be appropriate to discuss the basis of the experimental methods that
were used as well as the scientific theory on which the work is based. Usually a well-written introduction makes use of written resources
in the form of scientific books and papers, which must be listed in the references cited and footnoted with the appropriate reference.

The Experimental Procedure section explains in detail exactly how the experiment was conducted. It should be possible to reproduce
the experiment using the information found in this section. If standard procedures are used and not explained in detail, a reference should
be given. A list of materials and equipment is often a useful component in this section. It includes all chemicals used, including the
concentrations of solutions and all special equipment.

The Results section includes the data that were obtained in the experiment together with an explanation of the data. Often it is
useful to organize the results of the experiment in tables, and sometimes graphs are required as well. All tables and figures should be
titled and numbered. All columns in tables and axes of graphs, should be carefully labeled, not omitting units. If calculations have been
performed, the equations used should be clearly indicated and enough information about the calculations should be included so that they
can be clearly followed. The precision and accuracy of the results should be calculated by standard statistical methods if appropriate to
the experiment.

The Discussion / Conclusions section contains the thoughts of the experimenter about the significance of the work performed. Each
part of the experiment should be discussed. Numerical results should be evaluated, and the meaning of any statistical calculations explained.
The success of the experiment should be evaluated by referring to the objective of the experiment as presented in the introduction. Was
the experiment successful? Were the objectives met? What is the overall significance of the experiment?

The Literature Cited section lists all the references used in preparing the report. This section is the most formal in its format. It
is important to adhere to the style used. Each scientific journal has a slightly different style that contributors must follow to the letter.
Student reports may also be required to follow a certain form. The best way to write this section is with the help of an example. Often
college courses use scientific journals as models. The Journal of Chemical Education, Analytical Chemistry and the Journal of the American
Chemical Society are examples of chemical journals that have been used in this way; the Journal of Organic Chemistry is often used in
organic chemistry courses. When giving references, it is important to notice carefully all words that are set in italics or boldface in the
example references. Typesetters use different fonts for italics and boldface that are difficult to reproduce when typing or handwriting,
though many word-processing programs are able to reproduce them. Words that are set in italics can be indicated by an underline. Boldface
can be represented by a wavy underline.

Typically, a reference to a book appears as follows:

Reid R.C.; Sherwood T.K. Prausnitz J. M. Properties of Gases & Liquids; McGraw Hill: NY. 1977

A reference to a scientific journal follows this general form:

Lee L.G.; Whiteside G.M., J. Am. Chem. Soc . 1985, 107, 6999.

An example of a laboratory notebook

http://www.uic.edu/classes/chem/clandrie/CHEM112/syllabus/syllabus.html#example
http://www.dartmouth.edu/~chemlab/info/notebooks/sample.html
http://www.rod.beavon.clara.net/lab_book.htm
http://www.chem.purdue.edu/courses/chm25701/reports.html

8
9
10
IV Grading Rubric for Lab Notebook and Post-Experiment Write-up

Emphasis on the lab this semester is on how you carry out the experiment and the interpretation of the experimental results. The quality
of your work as demonstrated by your lab notebook (i.e., how well you record your data in table form, the thoughts in your discussion, and
in general the overall quality of your report) accounts for the majority of your grade. Although your report is important, your technique is
also part of your grade. Remember that you should always wear your safety glasses during lab. Failure to do so will result in lab technique
point deduction. Always wear your safety goggles once your locker is open. You may safely remove your goggles when the last person in
class has closed his/her locker.

Timelines and deadlines: All written work MUST be done in the notebook. Your laboratory notebook is YOUR responsibility. If you forget
to bring your lab notebook to class you will not be able to work in the lab. The original copies (top page of lab notebook) will be turned in,
the carbonless second page copy will remain in your lab notebook. Before beginning each experiment, you must have written an introduction
for the experiment in your notebook. If you do not have the pre-lab (introduction and procedure) complete, you will not be allowed to start
the experiment. The experimental procedure schedule for the day must be completed before starting the experiment unless otherwise
stated. The observation and data must be documented at the time experiment is being conducted, even if it consist of only a few
data points. The original copies of data and the observation section MUST be turned in BEFORE leaving the lab.

The original copies for the calculations-, discussions-, conclusions- and answers to the post-lab questions are due on the due-date of the
experiment. The write-up must be turned in at the beginning of class of the due-date (See lab schedule handout). If it is turn in after
this time, at best a 20% deduction will be imposed on the grade for the report at worst, you may not receive credit. In addition, for every
regular class meeting the report is not turned in, an additional 20% will be deducted from the report. If the report is not turned in after
two weeks (one week for summer session) of the due date, the report is given a score of zero.

General Guidelines: All work must be done in black or blue non-erasable ink. The use of correction fluid (such as white-out) is not
permitted (5-pt penalty). Data may not be photocopied. While discussion and exchanges of ideas is permitted, your lab write-up should be
done independently from your lab partner. DO NOT PLAGIARIZE.

The format on keeping a laboratory notebook is given in the next few pages. Please read this and adhere to the regulations. Early in the
semester the format will be graded thoroughly so please adhere to the format outlined below. I will follow these guidelines to the letter
in grading laboratory reports. Remember that all work should be recorded in the lab book directly, no scratch paper allowed. In the
procedural section, don't just write in your notebook— "refer to page # of the lab manual", a pictorial flowchart is required in this section.
This will be discussed in our first experimental meeting.

Start with the table of content. All pages must be referenced in the table of content with the table updated as entries are added to the
lab notebook. All entries must be in ink and no data entered is ever erased. The format is provided below and should be adhered to
throughout the course. Remember to begin all new projects on a new page. Skip pages only to follow the guidelines above. Depending on the
number experiments in the course it might be best to use two lab notebooks for this course since many of the experiments will overlap.

Keeping a Laboratory Notebook: The general guidelines was previously mentioned above. This outlines steps specific to this course.
One of the most essential skills a scientist need is the ability to keep a proper laboratory notebook. This is essential in documenting the
work that has been done, whether the information is needed later to write a paper or in order to submit a patent application based on the
experiments or simply to act as the archival record of the results. In this course the laboratory notebook you keep should be quite helpful
in studying for the quizzes and exams. At the discretion of your instructor, you may be allowed to use your notebook in the exam. It would
be advantageous to be diligent in your notebook upkeep.

One facet of writing the laboratory notebook that is generally difficult for students to decide, is how much information to write in the
notebook. The guideline to use is that a competent scientist should be able to reproduce the results of the experiment using only the
information in your notebook. It is usually better to err on the side of writing too much information than not enough. It is expected that
you will write in proper prose for the narrative portions of the notebook. A second facet is organization and neatness. A portion of your
grade on each experiment will be based on how good a job you do in organizing your notebook. If I cannot read what you wrote I will most
likely assume that it is incorrect and may ask you to resubmit your report. If you do not have legible penmanship it would be best to slowly,
and meticulously print your entries.

Table of Content: The following format for the laboratory notebook will be used in this course. The first 4-5 pages of the notebook are
for the table of contents. The table of contents should include the experiment number, the title, and the page of which the work for that
experiment begins. The table of content should be updated every time an entry is made in the notebook.

Header: For each experiment, the top margin of each page in the notebook should have 1) name of person who made the page entry, 2) the
title of the experiment, 3) your section number, 4) the date the work on the page was performed, 5) and the names of any lab partners.

11
INTRODUCTION
Objective, Background Info, Procedure and Safety and Prelab Questions: For each experiment the notebook should include the following
sections: Objective, background information, procedure (pictorial form) and standard operating procedures directions (SOPs) for
instruments that are to be deployed, chemical disposal and safety information.

1. Objective: The objective state why the experiment is being performed, i.e. the goal of the experiment. ALWAYS START the
objective as a complete sentence. In other words, do not start your prelab discussion with "To determine the concentration of...." .
The objective should be brief and to the point and should start out as "This experiment is to....".

2. Background: The background information provides the theoretical principles, which form the basis of the experimental method. The
background information should be written in your own words and not copied from this lab manual. Any pertinent balanced equations or
mathematical equation should also be included in this section. Add any other information you believe is necessary to bring your audience
up to date on the experiment.

3. Procedure: Next is the procedure. This does not mean that the procedure is copied verbatim into the laboratory notebook; rather a
reference to the procedure should be made followed by a pictorial flow-chart showing the steps in the procedure. Sketching an
experimental set-up or unusual equipment is very useful in reproducing the experimental procedure. Changes to the published should also
be included in this section.

4. Safety: The last section of the introduction section is the chemical disposal and safety information. Safety is of paramount
importance in the chemical laboratory. In order to raise awareness of any hazards associated with the chemicals or procedures used in
the experiments, warnings should be written in the lab notebook. Similarly, in order to be environmentally conscious chemical material
used should not be released to the environment, i.e. poured down the drain. Whenever possible, Green Chemistry should be practice
throughout this course. Review the 12 Principles of Green Chemistry at http://www.epa.gov/gcc/pubs/principles.html. In each
experiment, you will be given directed instructions on the proper method to dispose of chemical waste. If you are unsure about the
correct disposal procedure, ask your instructor or lab technician for guidance.

5. Prelab Questions: The last part of this section is the prelab questions assigned for the experiment. Do not write the answers for
these questions in your background narrative, instead, write out a separate section and answer with the question embedded in your
answer. For example, if the question is "Why is it necessary to standardize the titrant before the titration experiment"? An
appropriate answer would be, "In this experiment, it is necessary to standardize the titrant with KHP in order to know the precise
concentration so that the equivalent number of moles of the titrant can be used to analyze the analyte". Notice how the question is
embedded in the answer (in italics). Finally, be sure your answer is complete, otherwise, you will not receive full credit, if any.

Since the lab notebook are of the carbonless copy type, the original pages containing these sections should be turned in before class begins.
Something must be turned at the end of each lab experiment. Not turning in any data or observation means you were absent that day and
you will not receive credit for that day's work.

DATA & OBSERVATIONS

6. Data and Observations: The data / observations section is being written when carrying out the experimental procedure. The written
observation notes should be detailed enough that someone else could repeat the experiment simply by reading the notes. In general, it is
always a good idea to record more details than too few details. Important items to notice are the color changes, gas evolution, experimental
difficulties, etc.. that occurred during an experimental procedure. As the experiment is being conducted observations and numerical results
(data) should be entered directly in the lab notebook at the moment the data is collected and not a minute later. Raw data should never be
written on paper other than the lab notebook. That means the data should not be written on the lab manual or textbook. There is a
5pt penalty for each time this rule is violated or 20% penalty in your lab report. If the violation is egregious, a zero will be given for the
lab technique score. Data should always be entered in the lab notebook. The data should be organized into tables in a logical fashion so
that they are easily found when needed for calculations. Numerical data should be recorded with the correct units and precision. Try to
keep attachment or computer printout to one page and attach to the notebook via clear tape (no staple). A description of the attachment
should be entered in the lab notebook.

As mentioned already, the data / observation section is turned in before leaving class. That is, data / observation notes for all experimental
data collected on a particular day, must be submitted before leaving class. Let me stress again, if you are doing any part of the experimental
procedure during another class session, you are required to turn in your lab notebook page(s) of your data/observations for that day. DO
NOT, DO NOT, DO NOT, ever, ever, ever, write your data in a separate sheet of paper or in the this lab manual. You will automatically
receive a 5pt deduction per incident in your lab write-up report if you are caught writing your data and observations other than
your lab notebook. If you are collecting data digitally, be sure to write out the key data from the printout in your notebook at the time
the data is being collected. You never know if the computer will crash or some unexpected malfunction occurs with the computer. Do not
become too dependent on technology to store your data... a hand-written copy should always be kept in your laboratory notebook, after all,
that is the primary function of a lab notebook. All computer printouts should be properly labeled and a description of the printout should
be described in the notebook. Size the printout so that it fits a full 8 x 11" page.

Upon the discretion of your instructor, you will ask you to turn in a data card /result card for certain experiments so that the instructor
can monitor your progress and accuracy. You might also have to upload this information online via Blackboard. If required, your instructor
will provide you more information on this procedure at the appropriate time. You should never cut-and-paste the content of the data card
and use it as your table of your results in your notebook. You must hand write the entries in your notebook in pen.

12
RESULTS, CALCULATIONs and DISCUSSION
7. Results and Calculations: After leaving the laboratory the process continues. The next step is to try to make sense of the data that
was collected. In this section the data are manipulated in order to obtain the answers to the question posed in the objective. First organize
your raw data such that all the information you will need to calculate your results are found organized in a data table. In this section, you
should go back and organize your raw data that was entered in your notebook. If available, you can use the instructor's datasheet to help
in your organization. Next you should include key equations or provide the formulas that will transform the raw data to meaningful results.
You should include a complete sample calculation in this section showing how data is used in your calculation. If you are using excel to do
the bulk of the calculations, show the layout of the excel spreadsheet and the formulas for important cells in the spreadsheet. If you are
using excel for the statistical analysis, include the statistical function that is used in your description of how the values were obtained.
Described and formulas if the statistical calculations is new by providing a description in your notebook. If graphs are generated, be sure
to have a title for each graph with the axis properly labeled. A legend should include the meaning of the data points. If LINEST is used
for the linear regression, the complete 3x6 matrix (with labels) should be part of the graph and in the result table. Finally, you should take
the final results and present it in an organized table, highlighting the final numbers as requested in the lab write-up directions for that
experiment. In other words, the final results should be summarized in an “Table of Results” that is easily followed and properly labeled.
A clear, organized, delineation of raw data to results (including statistics) must be presented in this section.

Computer printouts should only be turned in if the instructor request the printouts, otherwise summarize the results. If you turn in the
printouts, organize the data and then attached it as an appendix to your report. A description of the printout should include in this section
as well. All printouts should be properly label. Do not confuse the computer printout with results that must be included in this section.
Some numerical printouts should not be turned in, especially if it is simply nothing more than pages and pages of numerical values. A good
rule of thumb is to contain the printout to one page. Talk to your instructor if you are unsure how to do this. If the printout is longer than
two pages but less than five, it is recommended to include it as an appendix. If the computer-generated table is greater than 5 pages, you
will need to condense it to fewer pages or leave it out.

8. Discussion and Conclusion: The next to the last section of the notebook is the discussion /conclusion section. This usually has two
parts. The discussion should speculate on the significance of the results that was found in the "results / calculation" section. The discussion
should also address if the results are what is expected or if an unexpected result was discovered. Finally the statistical analysis should
also be addressed in this section, i.e., state what part of the experimental procedure introduce the greatest error and comment on how
the errors (including any errors you made personally) affected the experimental result. The conclusion section should simply state the
final result, which pertains to the goal of the experiment.

9. Post-Lab Questions: All post-lab questions is answered at the end of your report. This should be written as a separate section do not
answer these questions as part of the lab discussion otherwise you will not be given credit for this section. You can use the post-lab
question as talking points but you will need to write out a Post-Lab question section. As in the prelab question section, you should give an
answer that has the question embedded in it. See the pre-lab question section above for more information on how to complete this.

10. Overall Presentation: In the lab, your instructor will be noting if you are following "good lab procedures" (GLP). This means you are
conscious of safety, are meticulous handling chemicals, dispose of waste properly and are tidy in your work area. Your demeanor when
conducting lab should be of a professional manner and one in which you are prepared to carry out the experiment. All part of your notebook
should be complete and turn in on time. When recording data, the observations are detail and the numerical entries are organized with the
proper units. The calculations should be easy to follow and arrange so that the instructor effortlessly follows along the math operation.
The discussion should be coherent and the talking points should center around the objective of the experiment.

11. Laboratory Techniques: Safety is of paramount importance. If you are not safety conscious when conducting lab, this portion of
your grade will reflect that. In addition to safety, be conscious of waste disposal and chemical handling. Finally, the accuracy and precision
of your result is a good indicator of your laboratory skills and technique. If your results are not accurate, nor precise, then your lab
technique score will reflect this in your report grade.

13
 Experiment Lab Notebook Write-up Criteria
General Chemistry (II) 201
Required Assignments: Students are required to perform assigned laboratory experiments, alone or with a partner. Before any lab period
and before the class begins, you should have already read the lab experiment and have the pre-lab assignment ready to submit. Reports
consist of observations made during the experiment, calculations and interpretation of your observations. You are required to answer all
follow-up questions concerning the concepts studied in each experiment. All work should be recorded in your lab notebook.

# CRITERIA (Tentative point distribution - may change depending on experiment) pts %

0 Quiz / Homework 5 – 10 %
1 Objective of Experiment
2 Background information (Math relationship used in study, pertinent chemical reactions, graph to be generated)
3 Procedures
• Short outline of procedures in Expt. • Flow chart pictorial of procedures. • Procedural changes. 10 -15%
• Information (data) to be recorded during expt. (Table template form.)
4 Safety precautions and disposal information.
5 Prelab Questions. This part may be part of the Homework/Quiz point distribution.

This portion of the report should be turned in before the start of lab class (prelab discussion).
6 Data and Observation
• Observation
• Detailed account of what was observed during the experimental procedure.
• Balance chemical equations; all chemical reaction which occurred during an experiment should be written in
this section. Then it should also be written in the discussion portion of the report.
• Data 15 -25%
• Data in table form with correct significant figures, precision and units for each entry. Data should always be
recorded in an organize fashion.
• If you worked for that period, you must have some form of documentation of what you did for that period.

This portion of the report should be turned in before you leave the laboratory.
This is true no matter how little data you collected on that day.
7 Calculations & Results
•Calculations
• Sample calculation shown • Statistical analysis of data and result (if applicable)
• Results 20 – 25%
• Result(s) in table form. • Clear delineation of how data is used to get the final results.
• Data card and result card to the instructor (if necessary)

In this section accuracy of results are very important as well as detailed calculation showing how the result
was obtained. "Unknown" will also be included in this section.
8 Discussion / Conclusions
• Discussion
•A complete discussion should be written in this section. Talking points can be found at the end of each
experimental procedure from the lab manual. Each discussion should include the significance of the result(s)
and the meaning of the result of the experiment. All chemical reactions that occurred during the experiment 15-25%
should also be included here.
• Conclusion
• Summary of the goal of the experiment and how that goal was achieved in the experiment

This portion (Calculation and Discussion) is turned in at the beginning of class of the due-date
9 Post Lab Questions
• Post-lab questions from manual or class assignment
• Complete well thought-out answers with an explanation. No explanation, no credit.
5 – 10%
This portion (Post lab question) is turned in at the beginning of class of the due-date
10 Overall Presentation (of lab notebook)
• Lab technique during lab e.g., class preparation, safety glasses precautions and leaving the laboratory clean.
• Lab report e.g., headings of each page of notebook including- name, title, lab partner, date and section #.
• Legibility of report: ease of readability of written work and clear delineation of calculations. 10%

The overall impression is important.

11 Lab Technique 5%
• Safety conduct, chemical handling and precision of work, sound statistical analysis, conclusion of results.
Total (This total may be adjusted depending on lab technique and student conduct in the experiment) 100%

14
 STATISTICAL TREATMENT OF EXPERIMENTAL MEASUREMENTS

Whenever a quantitative measurement is made, the value obtained will differ from the "true" or actual value due to the occurrence of
measurement errors. Moreover, there will be some uncertainty in the measured value due to the limitations placed on its precision by the
measuring device or method. In order to determine how good an estimate the measured value is of the true value, statistical methods are
employed.

The errors that result in the measured value, differing from the actual value, may be classified as either of one of two types:
SYSTEMATIC ERRORS or RANDOM ERRORS. Systematic errors result from instrumental miscalibration, improper experimental design,
or consistent operator bias. Such errors will result in the measured value being reproducibly higher or lower than the actual value.
Systematic errors may result in a constant offset (as for a thermometer which reads 2 °C high at all temperatures) or a relative percent
error (as for a balance which shows the weight of 10.000 gram standard to be 10.080 grams and a 1.000 gram standard to be 1.008
grams, i.e., giving results which are 0.80 percent too high). Since systematic errors cannot be dealt with by statistical means, they must
be eliminated.

Systematic errors may be detected using 1 or more of 4 general approaches. These are analysis of standard samples, independent
analyses, blank determinations, and sample size variation. The analysis of a standard sample of known composition allows comparison of
the measured values to a known actual value. If the measured values are consistently higher or lower than the actual value then a
systematic error exists. Unfortunately it is not always possible to obtain a standard sample, which closely duplicates the unknown sample.
This limits the applicability of this approach. In independent analyses, the same sample is analyzed by two or more different experimental
procedures. These procedures should be completely different from one another with regards to instrumentation employed and chemical
or physical properties utilized. By comparing the desired method with a method of known reliability the presence of systematic errors
can be detected. Blank determinations involve performing the method in the absence of the sample. Any reagents that are used in the
blank are subtracted from the amounts used in the actual analysis. In the variations of sample size method, the results are examined for
systematic increases or decreases that can be correlated with sample size.

Once detected, systematic errors must be eliminated or compensated for. Instruments can be calibrated, operator errors are minimized
by training, care, and self-discipline, the procedure may be revised, or a constant factor may be added or multiplied to the result.

Random errors result from insufficiently controlled variations in measurement conditions. Random errors can be minimized by careful
experimental design and operator technique, but they cannot be eliminated entirely. Fortunately random errors usually result in the
measured values being distributed about the actual value in a normal distribution or bell-shaped curve.

Initially we will be concerned with cases where we have performed 2-5 trials under the same conditions with the same materials. The
MEAN or average of such a data set is merely the sum of the values divided by the number of data points: x = (S x)/n. We will use
the mean to represent the best-measured value for the unknown quantity, since it depends upon all the trials instead of just one. This
approach is valid due the Central Limit Theorem.

It is not enough to obtain just the mean of the data. Some estimate as to the uncertainty or error of the mean is needed. When a series
of measurements of the same experimental parameter are conducted, the quality of the data depends upon both its PRECISION and
ACCURACY. Precision relates to the degree of scatter in the data, with less scattering equaling greater precision. For example, a set of
data for the weight of an object of 1.307, 1.308, 1.309, and 1.307 grams is more precise than a set of 1.300, 1.316, 1.305, and 1.310
grams. Accuracy relates to the difference between the measured value and the true value. Both of these data sets would have the same
accuracy as they have the same mean value.

Calculated precision values can be expressed either in absolute or relative terms. The most common methods for calculating absolute
precision are average deviation and standard deviation. Average deviation are found by finding the absolute values of the difference
between each data point, and the mean, and then taking the average of these deviations. For example, in the second data set above the
mean is 1.308 grams. The deviations are:

|1.308 - 1.308| = 0.008 grams

|1.316 - 1.308| = 0.008
|1.305 - 1.308| = 0.003
|1.310 - 1.308| = 0.002

The average deviation is ( .008 + .008 + .003 + .002)/4 = 0.005 grams.

15
In the real world we only rarely have a large number of measured values to work with. It is much more common to have 3-5 values.
Moreover, for unknown samples the true value is not known. Another measure of the absolute precision is the standard deviation:
2
# &
∑%$ x − x ('
σ=
n−1

While this expression is the formal definition of s, it is easier to calculate it from the following formula:
$ 2 '
&
%
(∑ x ) − (∑ x) /n)(
2

σ=
n−1

It is often more informative to express precision in relative terms. Here we relate the size of the deviation to the magnitude of the
measurement. An average deviation of 0.001 grams is a small uncertainty compared to a measured value of 10.000 grams but quite large
compared to 0.010 grams. We calculate relative deviation according to the formula
(absolute precision ) x (factor)
mean value

Thus for the above data set the relative precision expressed as a percentage is
0.005grams x 100
= 0.4%
1.308 grams

We can also express relative deviation as parts per thousand (ppt) by making the factor 1000, parts per million (ppm) using a factor of
1,000,000, and so on.

An alternate method for conveying the relative uncertainty in a value is to use the significant figure convention. Here we assume that all
of the digits in a number are certain except the last one, which has an uncertainty of +1 unit. The significant figure convention is
discussed in detail in your textbook.

Accuracy may also be calculated in absolute or relative terms. Absolute error is the difference between the measured and the accepted
values. Suppose the true or accepted value for the weight is 1.311 grams. Then the absolute error E is

= 1.308 - 1.311 = - 0.003 grams

The relative error is found by an analogous calculation as was used for relative precision. Here the relative error is

−0.003 grams x 1000

relative error = = −2ppt.
1.305 grams

Often we wish to express this as a percent error.

" (true value − experimental value) %

%error = $$ ' ∗ 100
'
# true value &

Example Suppose a student has dissolved solid NaOH in a 500 mL volumetric flask and then titrated it with standardized HCl in order to
determine the molarity of the resulting basic solution. (This is necessary because NaOH (s) is hygroscopic and some of the mass of the
solid used is undoubtedly H2O.) Three 25 mL aliquots of the basic solution were titrated using 12.75, 12.80, and 12.71 mL of 0.2000 M

HCl solution. Since M A x VA the three experimental values for the molarity of the basic solution are 0.1020, 0.1024, and 0.1017 M.
MB =
VB
The mean value is

X=
(0.1020 + 0.1024 + 0.1017) = 0.1020 M
3
The standard deviation of this data set is " 2 %
x values x2 values (
#
) ( )
$ 0.0312327 − 0.3061 /3'
&
0.1020 0.010404 σ x2 = = 1.4833•10−7
2
0.1024 0.0104858 σ x = 3.85 •10−4
0.1017 0.0103429
S 0.3061 S2 0.0312327

16
The relative standard deviation is: 1000 x 3.85•10-4
relative std deviation= = 3.8 ppt.
0.1020
If the true value of the molarity is 0.1015 M, then the absolute error E is

= (0.1015 - 0.1020)M = -0.0005 M

The percentage error is % error = [(0.1015 - 0.1020) / 0.1020] • 100 = -0.49 %

Sometimes in a data set there will be one value that appears to be anomalous, e.g., 15.25, 15.28, 15.30, and 16.34%. The first approach to
this situation is to ascertain whether there is a valid experimental reason to delete this point, such as an error in calculation or a
procedural error in the analysis itself. If this is not the case then the validity of the point can be established by using a Q-TEST:

(Suspect Value-Nearest Value)

Q=
(Suspect Value-Furthest Value)

If the absolute value of Q exceeds the value in Table 1 for a given confidence level then the point may be rejected. Otherwise. the point
must be kept in the data set. Using the above data set

(16.43 - 15.30)
Q= = 0.96
(16.43 - 15.25)

For 4 trials the 95% Q value in the table is 0.85. Since 0.96 > 0.85 we may reject this value with 95% confidence.

TABLE I
REJECTION QUOTIENT
Number of Q-Value
Trials (90%)
3 0.94
4 0.76
5 0.64
10 0.41

Most instrumental methods are based upon calibration data obtained by measurements performed on a series of standards containing
known concentrations of the analyte. Plots of concentration versus experimental observable are made. The "best" straight line through
the points is then determined by linear regression. We will consider only the simplest case, called the METHOD OF LEAST SQUARES,
which applies when there is a linear relationship between the analyte concentration and the measured variable. The method of least
squares depends upon two assumptions: that a relationship of the form y = mx + b exists between the measured observable (y) and the
analyte concentration (x), and that the error in x is negligible compared to the error in y. The line generated by the least-squares method
is the one that minimizes the squares of the individual vertical displacements, called residuals, from the line. A residual q has the form q
= [y1- (m + bx1)], and is thus a measure of the difference of the experimental value for y (y1) and the value for y calculated from the line

(m + bx1). This method minimizes the sum of q2, hence its name. The value of the least-squares method is that the slope and intercept of
the line are obtained as well as the standard deviation for an analysis based upon this line. Thus, from the measurement of y for an
unknown sample we can calculate both a value for x and its standard deviation using this method.

In this course we will use computer programs to generate the best fitting line through a set of data points. The program we use is based
on the method of least squares described above.

Reference:
1. http://ull.chemistry.uakron.edu/analytical/Statistics/
2. http://science.widener.edu/svb/stats/stats.html

17
18
 Laboratory Safety 8/18 –FG

The safety of yourself and your classmates is of paramount importance during laboratory. Safety regulations must always be observed as it only
takes one accident to cause blindness or serious permanent injury. Safety goggles must be worn at all times. After the first day of lab ten points
will be deduced if you come to lab without your safety goggles. If you remove your safety goggles when lab is being conducted your instructor will
give you a verbal warning once, the second time 10 points will be deduced, and a third offense will result in your being asked to leave the lab and an
additional 20 pts deduction.
In the laboratory, the chemist works with many potentially dangerous substances and equipment. Yet, with constant alertness, awareness of
potential hazards, and some common-sense precautions, laboratory operations can be carried out with a high degree of safety. The most general
rules for safety laboratory operations are: be alert - stay alert, and take the trouble to understand what you are doing and the potential hazards
associated with the operation you are performing.
Important Changes from District Risk Management Department
In order to mitigate potential accidents in the instructional laboratories, the SDCCD, Risk Management is taking a more active role and adopting a
new chemical hygiene plan (CHP) that is much more strict than previous practice. These new requirements will be implemented starting Fall 2017.
Attire and Personal Protective Equipment (PPE):
1. Whenever in a lab (even for dry labs), the following proper attire is required: closed-toed shoes and pants that go down to the ankle.
2. When working with chemicals, splash goggles (not glasses) and a lab coat that goes to at least the knee are required. Long hair must be tied
back. Refrain from wearing fluffy clothing. This rule applies to all in the lab.
3. Student lab coats must be 100% cotton with either snap or knot buttons to allow for quick removal. These will be available at the bookstore for
October for $20. Students can purchase their lab coats from an outside vendor, but it must meet the above requirements.
4. When working with chemicals and washing glassware, nitrile gloves must be worn. When leaving lab or contacting something that should not be
contaminated (i.e. keyboard, pen, pencil, calculator, etc.), gloves must be removed and disposed of in the broken glass container. Gloves must
also be removed when they become visibly soiled. *Glove usage will be discussed during check-in.
Conduct and Behavior in Lab
5. Never work alone in the laboratory - someone should be in the room with you at all times. No horseplay in lab.
6. Do not perform any unauthorized experiments.
7. You should immediately sweep up spill taking place on the balance.
8. Never throw matches, litmus or any insoluble solids into the sink.
9. Clear work area and lab at the end of lab.
Good Lab Practice and Safety Practice
10. Learn the location of the nearest eye fountain, fire blanket, safety shower, first aid-kit, broken glassware trash-bin, broom and dust
pan, campus (police) phone. Your instructor will update you with any other safety equipment you will need to familiarize yourself with.
11. De-Ionized water may be obtained through the gray faucet near the first two sink. (Generally, it is good lab technique to do a final
rinse with de-ionized water when cleaning glassware
12. Use fume-hood when working with poisonous or offensive gases/fumes, likewise when working with flammable/ explosive materials.
13. Never pour anything back into a reagent stock bottle - take out only as much as you will use.
14. Never pipet anything by mouth - especially toxic or corrosive substances.
15. Be sure to label all chemical containers correctly.
16. Never heat organic solvent (alcohol, ether, benzene, etc.) in an open vessel over a flame. These solvents are highly flammable,
especially with an open flame - use a hot plate to heat liquids that should be in an open vessel when these operations are performed.
17. Never add anything (including water) to conc. acid - instead slowly add the acid to the other substance to avoid acid splashing.
18. Avoid using excessive amounts of reagents - 1 to 3 mL is usually ample for test tube reactions.
19. Never heat reactants in a fully closed system - be sure the system is open to the air to prevent a pressure build-up and explosion.
20. Avoid pointing the mouth of a vessel being heated toward any person, including yourself and the instructor.
21. Beware of hot glass tubing - it looks cool long before it can be handled safely.
22. Hold glass tubes and the thermometers in a towel when pushing them through rubber stoppers.
23. Do not heat thick glassware such as volumetric flasks, graduated cylinder, or bottles; they break easily with heat.
24. Do not lay down the stopper of bottle. Impurities may be picked up and contaminate the solution when the stopper is returned.
These are by no means the only safety precautions you should take when working in the laboratory, but instead it is a guide as to how you
can avoid some of the common hazards. Above all else, use common sense precautions such as cleaning-up after a spill, not picking up red-
hot objects, no horseplay in lab, etc. Students not in accordance with these guidelines must leave the laboratory. These guidelines are
more in line with what is encountered in industry. As such, these changes better prepare students when going on to the universities or
working in industry.

SAFETY STATEMENT: I am aware that there are hazards associated with being in a chemistry laboratory. I have been made aware of
the safety equipment available in S6-203 and how it is to be used. I have also been made aware of some common hazards such as: broken
glass, fire, acids, bases, and the poisonous nature of most chemicals. I will always wear my safety goggles during lab. I understand that
special precautions for individual experiments will appear in the lab manual in a section entitled "Safety". (Please sign below).

Signature Date

Print name CSID

19
Safety Quiz Name:_________________last _______________First
____ / 10 Score Chemistry-251 Date _____________________

Indicate in the space provided whether each of the following lab safety statements is True (T) or false (F).

1 __ It is okay to wear safety glasses while working in the laboratory with chemicals.

2 __ Before working on an experiment you must know the location of the fire extinguisher, first-aid kit, eye wash station and
other safety equipment in the laboratory.

3 __ Never eat, drink, or smoke while in the laboratory.

4 __ Never taste any chemicals in the laboratory. Consider all chemicals to be hazardous unless instructed otherwise.

5 __ Wear shoes at all times while working with chemicals in the laboratory.

6 __ If any chemicals contact your skin or eyes, flush immediately with water, and then notify the instructor.

7 __ Perform all reactions that involve gases with an unpleasant odor under a fume hood.

8 __ Never directly smell a gas or vapor; instead, waft the scent gas toward your nose using a cupped hand.

9 __ Never point the open end of a test tube toward yourself or your neighbor when heating a chemical.

10 __ Lubricate the rubber stopper hole with glycerol or water before inserting glass (i.e., thermometer) in stopper.

11 __ Pour acids into water --not water into acid-- because the heat of solution will cause the acid to splatter.

12 __ Do not use alcohol or other organic liquids near an open flame.

13 __ It is okay to dispose of all solutions including all organic chemicals down the sink.

14 __ It is okay to perform any unauthorized experiments.

15 __ It is okay to disregard the special safety precautions mentioned in each experiment.

16 __ The instructor must be notified immediately in case of an accident, but after the emergency has been addressed.

17 __ Read the experiment before each lab including: Objectives, Discussion, Procedure, & Pre-lab Assignment.

18 __ If glassware breaks while in use, it is okay to leave it alone, not to clean it up, and not to tell anyone.

19 __ Record your observations directly in your data table. Do not record data on loose, unbound, notebook paper.

20 __ It is okay to eat snacks or your lunch (dinner) while conducting the experiment in the laboratory.

21 __ Never place chemicals directly on the balance pan (without a weighing paper or weighing boat).

22 __ Never place a hot or warm object on the balance pan. Allow objects to cool to room temperature so as to avoid weighting errors.

23 __ Proper attire must be worn at all times, this includes shorts that is slightly above the knees.

24 __ When an experiment calls for water, use distilled (DI) water. When cleaning glassware, use tap water & rinse with DI water.

25 __ Return all community lab equipment to its original place, i.e., return ring stand to location under east sinks. Place excess solid
chemicals in a waste-crock or other designated waste container. Clean lab station upon completion of the experiment.

When this safety quiz is returned to you graded, note which items are incorrect and correct these by restating the question to the positive.

For example, the following statement is false.

All lab should be halted at 9:45PM so that there will be ample time to clean and everyone will be out the door at 9:55PM, when class is over.
To restate this statement to the positive the correct statement should be re-written as:
All lab should be halted at 9:35PM so that there will be ample time to clean and everyone will be out the door at 9:45PM, when class is over.
This statement is now true since the time has been changed to the correct time.

20
 ACTIVITIES

ACTIVITIES

ACTIVITIES

ACTIVITIES

21
22
01 Activity: Review of Basics
____ / 10 Score Name (last)____________________(first)____________________

1 Show your work in another sheet of paper and then fill in the blanks in the table.
Your answer could contain the right number of significant figures with the correct units.
Compound Molality Weight Percent Mole Fraction

A HF 20.0 %

B CH3CO2H 1.50 m

2. Fill in the blanks in the table. Your answer should contain the right number of significant figures with the correct units.
Compound Grams Grams Water Molality Mole Fraction of % concentration
Compound Compound

Na2CO3 40.5 155.0

C3H7OH 250. 2.55

NaNO3 555 0.0334

3. Potassium iodate reacts with potassium iodide and hydrochloric acid to produce iodine, water, and potassium chloride.

Write a balanced chemical equation for this reaction __________________________________________(Answer)

Determine the limiting reagent when 50.00mL of 0.0100M potassium iodate is treated with 1.00 g of potassium iodide and 10.00ml of 3

M hydrochloric acid. Calculate the amount of I 2 (grams) produced. ____________________Limiting reagent

______________________ mass I2

4. Consider the following chemical reaction: ____ KOH (aq) + ____ O2 (g) g ____ KO2 (s) + ____ H2O (l)

A volume of 525 mL of 0.500M KOH (aq) is combined with 500 mL of oxygen at 298 K and 750.0 mmHg.

Answer the following questions.

a) What is the balanced equation? Place Coefficients in the equation above.

b) How many moles of KOH before the reaction begins? ___________moles KOH

c) How many moles of O2 before the reaction occurs? ____________moles O2

d) Which chemical is the limiting reagent (if any) ? ______________ Limiting Reagent

e) What mass of KO2 (g) is produced? _____________________ mass of KO2

f) How many molecules of water is formed? ____________________ molecules of H2O

5. A flask contains 625 mL of 3.05 M nitric acid solution. What volume of 15.8 M HNO3 contains the same mole amount of HNO3 as
this solution?
_______________ volume HNO3

6. A sulfuric acid solution has a density of 1.73 g/mL and contains 80.0 percent H2SO4 by weight. What is the molarity of this
solution?
_______________ Molarity Sulfuric Acid

Note: If you rip this page from the lab manual, be sure to trim the edge. (Reminder from your lab instructor)

23
24
02 Activity: Penny Statistics1
____ / ____ Score Name (last)____________________(first)____________________

U.S. pennies minted after 1982 have a Zn core with a Cu over layer. Prior to 1982, pennies were made of brass, with a
uniform composition (95 wt % Cu : 5 wt % Zn). In 1982, both the heavier brass coins and the lighter zinc coins were minted.
In this activity, the class will weigh pennies and add to the pool of pennies that were already recorded. the data will be
analyzed to answer some of the following questions: (1) Do pennies from different years have the same average mass? (2)
Does the average mass of pennies change with age? (3) Do the masses of the pennies follow a Gaussian distribution?

1. Gathering Data
(a) If instructed each student should collect and weigh 20 pennies to the nearest milligram. In addition to the weigh,
record the city in which the penny was minted and the condition of each coin. Use the following grade:
(P) Poor - Barely identifiable; must have date and mint mark, otherwise pretty thrashed.
(Fa) Fair - Worn almost smooth but lacking the damage Poor coins have.
(G) Good - Heavily worn such that inscriptions merge into the rims in places; details are mostly gone.
(VG) Very Good - Very worn, but all major design elements are clear, if faint. Little if any central detail.
(Fi) Fine - Very worn, but wear is even and overall design elements stand out boldly. Almost fully-separated rims.
(VF) Very Fine - Moderately worn, with some finer details remaining. All letters should be readable. Full, clean rims.

Record your data in your notebook and add it to the pool of coins that were already recorded. The pooled data may also
contain a number of brass coins and a similar number of zinc coins from previous classes. Instructions are given for a
spreadsheet so that MS Excel statistic calculations can be carried out. Take the newly acquired data and compile a
spreadsheet and present your result to complete this activity. Be sure to answer all questions found on page 5 of this
activity.

(b) Sort the pennies into each of their

calendar year. Take the data for all
the pennies and sort it by year by
copying and pasting the pennies from
the original list to column of each year.
Each column should list the masses of
pennies from only one calendar year.
Use the spreadsheet "sort" function
to sort each column so that the
lightest mass is at the top of the
column and the heaviest is at the
bottom. (To sort a column, click on the
column heading to select the entire
column, go to the DATA menu, select
the SORT tool, and follow the
directions that come up.)

(c) Next find the 1982 pennies. There will be two columns for 1982, in which both types of coins were made. Create two
other columns for just 1982 light (zinc) and heavy (brass) pennies.

2. Discrepant Data
(a) At the bottom of each column, compute the mean and standard deviation. Retain at least one extra digit beyond the
milligram place to avoid round-off errors in your calculations. Damaged or corroded coins may have masses different from
those of the general population. Discard grossly discrepant masses lying ≥ 4 standard deviations from the mean in any one
year. (For example, if one column has an average mass of 3.000 g and a standard deviation of 0.030 g, the 4-standard-
deviation limit is ±(4 × 0.030) = ±0.120 g. A mass that is ≤2.880 or ≥3.120 g should be discarded.)

(b) After rejecting discrepant data, re-compute the average and standard deviation for each column.

25
 3. Confidence Intervals and t Test

(a) Select the two years (≥1982) in which the zinc coins have the highest and lowest average masses. Select years with a
minimum of 10 data.

(b) For each of the two years, compute the 95% confidence interval. Use the t-test to compare the two mean values at the
95% confidence level.

(c) Are the two average masses significantly different?

(a’, b’, c’) Try the same for two years of brass coins (≤1982).

4. Distribution of Masses

(a). List the masses of all pennies made in or

after 1983 in a single column, sorted from lowest
to highest mass. There should be at least 300
masses listed. Divide the data into 0.01-g
intervals (e.g., 2.410 to 2620 g) and prepare a bar
graph, like that shown in Figure 1. Find the mean
" , median, and standard deviation (s) for all
coins in the graph. For random (Gaussian) data,
only 3 out of 1 000 measurements should lie
! outside of " ± 3s. Indicate which bars (if any)
lie beyond ± 3s. In Figure 1 two bars at the right Figure 1. Distribution of penny masses from the years 1982 -
1992 measured in Dan's house by Jimmy Kusznir and Doug
are outside of " - ± 3s.
Harris in December 1992.
!

5. Least-Squares Analysis: Do Pennies Have the Same

Mass!Each Year?
(a) Prepare a graph like Figure 2 in which the ordinate (y-
axis) is the mass of zinc pennies minted each year since
1983 and the abscissa (x-axis) is the year. For simplicity,
let 1983 be year 1, 1984 be year 2, and so on. If the mass
of a penny increases systematically from year to year, then
the least-squares line through the data will have a positive
slope. If the mass decreases, the slope will be negative. If
the mass is constant, the slope will be 0. Even if the mass
is really constant, your selection of coins is random and the
slope is not exactly 0. We want to know whether the slope
is significantly different from zero. Suppose that you have
data for 14 years. Enter all of the data into two columns of Figure 2. Penny mass versus year for 612 coins. Because
the least-squares spreadsheet. Column B (xi) is the year (1 the slope of the least-squares line is significantly less
to 14) and column C (yi) is the mass of each penny. Your than 0, we conclude that the average mass of older
table will have several hundred entries. (If you are not pennies is greater than the average mass of newer
using a spreadsheet, just tabulate the average mass for pennies.
each year. Your table will have only 14 entries.)

(b) Calculate the slope (m) and intercept (b) of the best straight line through all points and find the uncertainties in slope
(sm) and intercept (sb).

26
Use Student's t to find the 95% confidence interval for the slope: confidence interval for slope = m ± t sm (1)

where Student’s t is for n-2 degrees of freedom. For example, if you have n = 300 pennies, n-2 = 298, and it would be
reasonable to use the value of t (= 1.960) at the bottom of the table for n = ∞ (Use Student’s t table in your text). If the
least-squares slope is m ± sm = -2.78 ± 0.40 mg/year, then the 95% confidence interval is m ± t sm = -2.78 ± (1.960)(0.40) =
-2.78 ± 0.78 mg/year. The 95% confidence interval is -2.78 ± 0.78 = -3.56 to -2.00 mg/year. We are 95% confident that
the true slope is in this range and is, therefore, not 0. We conclude that older zinc pennies are heavier than newer zinc
pennies.

6. Does the Distribution of Masses Follow a Gaussian Distribution?

The smooth Gaussian curve superimposed on the data in Figure 1 was calculated from the formula

Now we carry out a χ2 test (pronounced “ki squared”) to see if the observed distribution (the bars in Figure 1) agrees with
the Gaussian curve. The statistic χ2 is given by

where yobs is the height of a bar on the chart, ycalc is the ordinate of the Gaussian curve (Equation 2), and the sum extends
over all bars in the graph. The calculations for the data in Figure 1 are shown in Table 1.

At the bottom of Table 1 we see that χ2 for all 21 bars is 43.231. In Table 2 we find a critical value of 31.4 for 20 degrees
of freedom (degrees of freedom = one less than number of categories). Because χ2 from Equation 3 exceeds the critical
value, we conclude that the distribution is not Gaussian.

It would be reasonable to omit the smallest bars at the edge of the graph from the calculation of χ2 because these bars
contain the fewest observations but make large contributions to χ2. Suppose that we reject bars lying >3 standard
deviations from the mean. This removes the two bars at the right side of Figure 1, which give the last two entries in Table
1. Omitting these two points gives χ2 = 30.277, which is still greater than the critical value of 28.9 for 18 degrees of
freedom in Table 2. Our conclusion is that at the 95% confidence level, the observed distribution in Figure 1 is not quite
Gaussian. It is possible that exceptionally light coins are nicked and exceptionally heavy coins are dirty or corroded. You
would need to inspect these coins to verify this hypothesis.

Table 1. Table 2.
Calculation of χ2 for Figure 1 Critical values of χ2 that will be exceeded in 5% of
experiments*

27
28
02 Activity: Statistics with Excel
____ / ____ Score Name (last)____________________(first)____________________

You can show your work on extra sheet but your final answer must be written on the original hand-out.
Reporting Your Results
1.(1 pts) Gathering Data:
(a) Collect and weigh enough pennies to the nearest milligram to provide a total set that contains around 6 00 brass coins
(b) Attach a table of masses, with one column sorted by mass for each year.
(c) Divide 1982 into two columns, one for light (zinc) and one for heavy (brass) pennies.

2. Discrepant data:
(a). List the mean ( " ) and standard deviation (s) for each column.
(b). Discard data that lie outside of " ± 4s and re-compute " and s .

3. Confidence intervals and t test:

(a) For !
the year ≥1982 with highest average mass:
! (= " ± t s / n ) = _______________
(b) 95% confidence interval !
For the year ≥ 1982 with lowest average mass:
95% confidence interval = _______________
(c) Comparison of means with t-test:
€
t calculated = __________
! t table = ____________
Is the difference significant? _____________

(a’) For the year ≤1982 with highest average mass:

(b’) 95% confidence interval = _______________
For the year ≤1982 with lowest average mass:
95% confidence interval = _______________
(c’) Comparison of means with t test:
t calculated = __________ t table = ____________
Is the difference significant? _____________

4. Gaussian distribution of masses:

Prepare a graph analogous to Figure 1 with labels showing the ±3s limits.

5. Least-squares Analysis:
(a) Prepare a graph analogous to Figure 2 and find the least-squares slope and intercept and their standard deviations.
(b) m ± sm = _________________
t95% confidence = ________ t 99% confidence = ________
95% confidence: m ± sm = ______________________.
Does interval include zero? ____________
99% confidence: m ± sm = ______________________.
Does interval include 0 ? ____________
Is there a systematic increase or decrease of penny mass with year? ____________

6.χ2 test: (Optional 5pts EC)

Write Equation 2 for the smooth Gaussian curve that fits your bar graph.
Construct a table analogous to Table 1 to compute χ2 for the complete data set.
Computed value of χ2 = ____________ Degrees of freedom = ____________
Critical value of χ2 = ____________
Do the data follow a Gaussian distribution? ____________
Now omit bars on the graph that are greater than 3 standard deviations away from the mean
and calculate a new value of χ2 with the reduced data set.
Computed value of χ2 = ____________ Degrees of freedom = ____________
Critical value of χ2 = ____________
Does the reduced data set follow a Gaussian distribution? ____________

1. T. H. Richardson, J. Chem. Ed. 1991, 68, 310. In a related experiment, students measure the mass of copper in the penny as a
function of the year of minting: R. J. Stolzberg, J. Chem. Ed. 1998, 75, 1453.
Note: If you rip this page from the lab manual, be sure to trim the edge. (Reminder from your lab instructor)

29
03 Activity: Chemical Equilibrium and Acid-Base
____ / ____ Score Name (last)____________________(first)____________________

You can show your work on extra sheet but your final answer must be written on the original hand-out.
Follow the following directions: For numerical calculations, show your complete work in a separate piece of paper, box your answer,
and then write answer in this worksheet.
1. Consider the following system at equilibrium: __CH4(g) + __C(s) + __O2(g) D __H2CO (g) DH = - 135.2 Kcal

Complete the following table. Indicate changes in moles and concentrations by entering I, D, N, or ? in the table.
(I = increase, D = decrease, N = no change, ? = insufficient information to determine)
Direction of shift, left, right or no Change in number of Change in molar
Change or stress imposed on change to re-establish, equilibrium moles concentration Chg
the system at equilibrium (After stress has been imposed) CH4 C O2 H2CO CH4 C O2 H2CO Temp
a) Add C

b) Remove CH4

c) Add H2CO

d) Increase O2 pressure

e) Decrease volume of reaction

vessel
f) Increase temperature

g) Add catalyst

h) 2.0 mol of O2 & H2CO are

added at the same time

2. For the reaction: H2 (g) + l2 (g) D 2 HI (g), Kc = 0.170, at 500.0 K.

a) What concentration of l2 (g) will be in equilibrium with [H2]eq = 0.040 M, [HI]eq = 0.150 M? ___________(Answer)

3. The solubility of CaCO3 at 25°C is 6.90 •10-5 M. The reaction is: CaCO3 (s) D Ca+2(aq) + CO3-2(aq)

a) Calculate the concentration of Ca+2 and CO3-2 at equilibrium.

_____________________ Ca+2 ___________________ CO3-2 (Answer)

b) Calculate the equilibrium constant for the dissolution reaction. (This equilibrium constant is also known as the solubility product.)

4. The value of Kc = 2.20•10-10 for the equilibrium: COCl2 (g) D CO(g) + Cl2 g)

If the concentration of Cl2 at equilibrium = 4.80•10-6M,

a) What are the equilibrium concentrations of the other two substances? [CO] = ___________(Answer)

[COCL2] = ___________(Answer)

b) What was the initial conc. of COCl2 ? ___________(Answer)

30
5. A 0.400 M HClO solution was found to have an H+ concentration of 1.10•10-4M. The reaction is: HClO (aq) D H+ (aq) + ClO-(aq)

a) Calculate the equilibrium constant for the ionization reaction (also known as the acid dissociation constant, Ka). ________(Answer)

b) Calculate the ratio ( D[HClO] / [HClO] initial)* 100 . This value is also known as the percent ionization (a).

___________(Answer)

6. At 1285°C the equilibrium constant for the reaction: Br2(g) D 2 Br (g) is Kc = 1.04•10-3.

A 0.200-L vessel contains an equilibrium mixture of the gases has 0.245g Br2 (g), what is the mass of Br (g) in the vessel?

___________(Answer)

7. Hydrosulfuric acid is a diprotic acid. Its two stages of ionization is shown below:

H2S (aq) D H+ + HS-(aq) Kal 5.70 • 10-8

HS- (aq) D H+ + S 2-(aq) Ka2 = 1.00 • 10-9

a) Calculate the concentration of HS- ion in a 0.222 M H2S solution [HS- ] =______________(Answer)

b) Determine the pH of the solution. pH = ______________(Answer)

c) Determine the S-2 concentration. [S2-] = ______________(Answer)

8. Methyl red is a common acid-base indicator. It has a Ka equal to 6.3•10-6. Its un-dissociated form is red and its anionic form is

yellow. a) What color would a methyl red solution have at pH = 7.00 ? Show your calculations and explain your answers (in words).

Hint: Determine the concentration ratio of methyl red and its conjugate.

9. Rank the following in order of increasing pOH and justify: 0.10M solutions of chloroacetic acid, carbonic acid and citric acid
Write out the order instead of placing 1, 2 ...

10. Rank the following in order of increasing pKa and justify: 0.10 M Mandelic acid, 0.20 M Maleic acid, 0.40M Malonic acid.
Write out the order instead of placing 1, 2 ...

31
Follow the following directions: For numerical calculations, show your complete work in a separate piece of paper, box your answer,
and then write answer in this worksheet.

11. Consider the titration of 20.00 mL of 0.250 M HF solution with 0.250 M KOH. Calculate the pH.after: 0.00, 5.00, 10.00, 19.00,
20.00 and 25.00 mL of base have been added. Sketch and label the titration curve for this problem.

Your answer here

Vol KOH 0.00-mL 5.00-mL 10.00-mL 19.00-mL 20.00-mL 25.00-mL

pH

14

12

10

0 0 5 10 15 20 25 30 35 40 45 50

32
33
04 Activity: Electrochemistry Basics
____ / ____ Score Name (last)____________________(first)____________________

Use the table of Standard Reduction Potentials in your textbook to help you answer the following questions.

1. Consider the following reaction as written:

Fe (s) + 2 Ag+(aq) g Fe+2 (aq) + 2Ag (s)

a. Write the line notation for the above reaction.

b. Write the half-reaction that occurs at the anode. Determine the E° for the half reaction.

c. Write the half-reaction that occurs at the cathode. Determine the E° for the half reaction.

d. Could this reaction be used as a battery? Calculate E° and justify your answer.

2. Consider the following half-reactions:

Cl2 (g) + 2e- g 2Cl-(aq) Eo = 1.36 V

I2 (g)+ 2e- g 2I-(aq) Eo = 0.535 V

Pb+2(aq) + 2e- g Pb(s) Eo = - 0.126 V

Cr+3 (aq) + 3e- g Cr (s) Eo = - 0.74 V

Mn+2 (aq) + 2e- g Mn (s) Eo = - 1.18 V

a. Which species above is the strongest oxidizing agent? Why?

b. Which species above is the strongest reducing agent? Why?

c. Which specie(s) can be oxidize by Pb+2(aq)? Calculate the voltage for this (these) process(es).

34
3. An electrochemical cell, which has the following line notation:
X(s) | X +n(aq) || Ag+(aq) | Ag (s) Eo cell = 1.1373 V
(Note that X is a chemical that you will need to identify with oxidation state. +n. Use the appendix in your text)

a. Write the half-reaction that occurs at the cathode and determine the Eo cathode.
(Use the symbol X for now if this is the reaction at the cathode)

b. Write the half-reaction that occurs at the anode and determine the Eo anode.
(Use the symbol X for now if this is the reaction at the anode)

c. Identify the X(s) | X +n(aq) half-reaction and determine the Eo for this reaction.

d. Sketch the electrochemical cell for this reaction, using lecture notes as a guide. Label the anode, cathode, each electrode
composition, ions in solution, direction of electron flow, and direction of ion flow in the salt bridge.

e. Calculate DGo for the reaction.

f. Calculate the equilibrium constant, Keq, for the reaction at 25°C.

g. Calculate E for the cell if the following concentrations are measured at 25°C.
[X+n] = 0.50M; [Ag+] = 0.20M

35
04 Activity: Electrochemistry Basics
____ / ____Score Name (last)____________________(first)____________________

Thermodynamic values are given in the appendix of your lab manual.

4. For the half-reaction: Pb4+(aq) + 2e- D Pb2+(aq)

Calculate the cell voltage, E, at 25°C if the concentration of Pb4+ is 0.5 M and that of Pb2+ is 0.1M. Hint: use the Nernst equation.

5. Calculate DG (in kJ) for the reaction: Cd + Pb2+ D Cd2+ + Pb

if the potential, E, of the cell was measured as +0.29 V.

6. A voltaic cell utilizes the following reaction and operates at 25°C.

__ Fe3+ (aq) + __H2 (g) D __ Fe2+(aq) + __ H+ (aq) (Note balance)

a) What is the emf of this cell under standard conditions? [0.771] V

(b) What is the emf for this cell when [Fe3+ ] = 0.53 M, PH2 = 0.25 atm, [Fe2+] = 0.012 M, and the pH in both compartments is 4.00.

[1.087] V

36
7. Alcohol levels in blood can be determined by a redox titration with potassium dichromate according to the redox equation:
C2H5OH (aq) + Cr 2O72-(aq) g CO2(g) + Cr3+ (aq)

What is the blood alcohol level in m/m if 8.76 mL of 0.04988M K2Cr2O7 is required for titration of 10.002 g sample of blood?

8. Use the half-reaction method to balance each of the redox reactions below. Note that these are under basic conditions.
After balancing the equations, answer the following questions for each reaction:
a) In the half reaction you wrote, which species is undergoing oxidation and which is undergoing reduction?
b) What are the possible oxidation states of chlorine in the reactions (i & ii) below?

1) Cl2 (aq) ® Cl-(aq) + ClO3- (aq) (basic conditions)

2) ClO-(aq) + CrO2 -(aq) ® Cl-(aq) + CrO42- (aq) (basic conditions)

37
05 Activity: Spectroscopy
____ / ____ Score Name (last)____________________(first)____________________

For all spectral analysis, show your complete analysis and provide evidence for your proposed structure.

Basic Spectroscopy
1. Determine the index of hydrogen deficiency for the following-

a) C8H7NO b) C4H4BrNO2 c) C21H22N2O2

2. Calculate the molecular formulas for possible compounds with molecular masses of 136, using the Rule of Thirteen.
You may assume that the only other atoms present in each molecule are carbons and hydrogens.
a) A compound with two oxygen atoms
b) A compound with two nitrogen atoms and one oxygen atom
c) A compound with five carbon atoms and four oxygen atoms

UV-Vis Molecular Absorption Spectroscopy

Reference: Google search key words: UV chromophores table
3 Draw the structural formulas that show a UV maximum at-
a) An acid, C 7H4O2Cl2 shows a UV with lmax = 242 nm.
b) An aldehyde C 8H12O, absorbs in the UV with lmax = 244 nm.

4 Predict the UV maximum for each of the following substances-

O O
H3C C CH3
CH3
O O
C C C
H2 C
N
H3C
H3C CH3
a) b) H

Reference:
Search “Woodward’s Rules for Enones”
https://chem.libretexts.org/Core/Organic_Chemistry/Spectroscopy/Visible_and_Ultraviolet_Spectroscopy/Empirical_Rules_for_Absorption_Wavelengths_of_Conjugated_Systems

Infra-Red Spectroscopy
5 In each of the following part of the molecular formula is given. Deduce the structure that is consistent with the infrared spectrum.
There may be more than one answer.

C9H12O

a)

C9H7N

b)

38
Nuclear Magnetic Resonance Spectroscopy
6 Determine the organic structure for the following. Provide as much evidence as possible for the structure you proposed.
.
a) The following NMR spectra are of mono-substituted aromatic hydrocarbon compound with the formula C10H14. The
chemical shift in the aromatic region is found between 7.1 and 7.3 ppm. Proposed reasonable structures.

b) Below are the NMR spectra of two isomeric carboxylic acids, C 3H5ClO2 . Proposed reasonable structures.

7. Using a correlation table for 13C chemical shifts, calculate the d for the carbons for the following chemicals.
CH3

a) CH3 b) HO c)

Mass Spectroscopy
8 The mass spectrum of an unknown halo-organic liquid shows a molecular ion peak at m/e = 78 with a relative intensity of 23.6. Suggest a
reasonable chemical formula and structure given the relative intensities of the isotopic peaks are as follow-

m/e: = 79 80 81
Relative intensities: = 0.79 7.55 0.25

39
Atomic Absorption Spectroscopy
9 The chromium in an aqueous sample was determine by pipetting 10.0mL of the unknown into each of five 50.0-mL volumetric flasks.
Various volumes of a standard containing 12.2 ppm Cr were added to the flask, followed by diluting each solution to volume.
.
Unknown , mL Standard, mL Absorbance
10.0 0.0 0.201
10.0 10.0 0.292
10.0 20.0 0.378
10.0 30.0 0.467
10.0 40.0 0.554

a) Plot the data

b) Derive an equation for the relationship between absorbance and concentration of standard.
c) Calculate the standard deviation for the slope and the standard deviation about regression in (b)
d) Calculate the ppm Cr in the sample
e) Calculate the standard deviation of the results in (d)

Fluorescence Spectroscopy
10 Quinine is one of the best known fluorescent molecules. The sensitivities of fluorescence are often specified in terms of the detection
limit for this molecule. The structure of quinine is given below. Predict the part of the molecule that is most likely to behave as the
chromophore and fluorescence center.
H3C
O

HO H

H H
N
N

11. The reduced form of nicotinamide adenine dinucleotide (NADH) is an important and highly fluorescent coenzyme. It has an absorption
maximum at 340nm and an emission maximum at 465 nm. Standard solutions of NADH gave the following fluorescence intensities:
Conc NADH, (umol/L) = 0.100 0.200 0.300 0.400 0.500 0.600 0.700 0.800
Relative intensities, I = 2.24 4.74 6.59 8.98 10.93 14.01 15.49 18.02

a) Construct a calibration curve for NADH.

b) Compute the least-squares regression parameters of a linear equation for the plot in part (a)

c) Calculate the standard deviation of the slope and the intercept.

d) An unknown exhibits a relative fluorescence of 12.16. Calculate the concentration of NADH

e) Calculate the relative standard deviation for the result in part (d)

f) Calculate the relative standard deviation for the result in part (d) if the reading of 12.16 was the mean of three measurements.
See, Chapter 4.9, Harris (8th Edition)

12. Why is spectrofluorimetry potentially more sensitive than spectrophotometry?

40
Spectroscopy Combination Spectral Analysis
13. Use the information provided to propose a reasonable organic structure for the halogenated alkane.

41
14. The compound has the formula C 4H8O.

The 1 H NMR spectrum shows a triplet at

9.8 ppm and the signal at 2.4 ppm is a
triplet of doublet. Suggest a reasonable
structure for the compound.
.

15. The compound has the formula C 3H6O2.

The UV spectrum of the compound shows
no maximum above 205 nm. The carbon
NMR spectrum shows peaks at 14, 60 and
161 ppm. The peak at 161 ppm appears as
a possible peak in the DEPT-90 spectrum.
.

42
43
06 Activity: Chromatography (Revised 08/18)

____ / ____ Score Name (last)____________________(first)____________________

For all questions, show your complete analysis and provide an explanation or justification.

Basic Chromatography
1. Consider a mixture of compound A, a somewhat polar liquid, and compound B, a somewhat nonpolar liquid. Tell which liquid, A and B, would

emerge from a chromatography column first under the following conditions and why:

a) A polar liquid mobile phase and a nonpolar liquid stationary phase

b) A nonpolar liquid mobile phase and a polar liquid stationary phase

2. The retention factor (or capacity factor), K of a compound is defined as K = ms/mM, that is K is the ratio of the masses of the

compound in equilibrium in the two phases. Show, from the information given in the corresponding chromatogram, that the expression

used k = (tR - tM) / tM is equivalent to this. Remember that for a given compound the relation between the retention time tR, the

time spent in the mobile phase tM (hold-up or dead time) and the time spent in the stationary phase ts, is as follow: tR = tM + ts

3. The efficiency of a gas chromatography column is measured by a parameter called plate height (H, mm), which is related to the gas flow

rate (u = mL/min) by the van Deemter equation: H = A + B/u + Cu, where A, B and C are constant. Prepare a spreadsheet with a

graph showing values of H as a function of u for u = 4, 6, 8, 10 20, 30,40,50, 60, 70, 80, 90 and 100mL / min. Use the values, A =

1.65 mm, B = 25.8, and C = 0.0236.

i) From your plot, what is the optimum flow rate for this column.

ii) What is the optimum plate height (H , mm) for this column.

iii) What are the units for the constants B and C?

4. Solvent passes through a column in 3.0 min, but solute requires 9.0 min.

i) Calculate the capacity factor, k'.

ii) What fraction of time is the solute in the mobile phase in the column?

iii) The volume of stationary phase is one-tenth of the volume of the mobile phase in the column ( Vs = 0.10 Vm).

Find the partition coefficient, K, for this system.

44
 Gas Chromatography

5 An injection of 3.00 microL of CH2Cl2 (density = 1.327 g/mL) gave a peak size of 3.74 cm3. The injection of 3.0 microL of an unknown

sample (density = 1.174 g/mL) gave a methylene chloride peak size of 1.02 cm 3. Calculate a response factor for methylene chloride and

the percent of methylene chloride in the sample.

6. A chromatogram reveals a resolution factor of 1.5 between two neighboring peaks, 1 and 2. If K2 = 5 and a = 1.05, and knowing that the

retention time of the compound 2 is 5 min, then:

a) Calculate the hold-up time of this chromatogram.

b) What is the width of the second peak at half-height, if the scale of the chromatogram is such that 1 min correspond to 1cm?
Use one of the following equations -

tr(2) - tR(1) 1 α - 1 k2 N α - 1 k 2 - k1
R = 1.177 ; R = N2 ⋅ ⋅ ; R = ⋅ ⋅
δ1 + δ2 4 α 1 + k2 2 α k1 + k 2 + 2

€
7.
What is the optimal flow rate for the. best separation of solutes?

The van Deemter eqn contains 3 terms describing three band broadening

mechanism.

i) Which term is zero (0) for an open tubular column? Explain.

ii) What is the physical meaning of the A, B and C term.

iii) For the graph shown, estimate the values of A, B and C.

Note that uo is the flow rate (mL/min) in the equation shown.

45
High Performance Liquid Chromatography

8 What type of HPLC should be chosen for each of the following separation application?

a) All mixture components have MW less than 2000, are molecular and polar, and are soluble in nonpolar organic solvents.

b) Mixture components have formula weights varying from very large to rather small and are nonionic.

c) Mixture components have formula weight less than 2000, are molecular and polar, and are water soluble.

9. What is the order of elution of the following acids from HPLC column whose stationary phase is of the type C18 while the mobile phase

is a formate buffer with a concentration of = 200 nM at a pH = 9.

Mixture:

1. Linoleic acid: CH3(CH2)4CH=CHCH2CH=CH(CH2)7CO2H

2. Arachidic acid: CH3(CH2)18CO2H

3. Oleic acid: CH3(CH2)7CH=CH(CH2)7CO2H

46
Experiment: Basic Lab Techniques in Analytical Chemistry Chem251 modified 08/2018

EXPERIMENTS

EXPERIMENTS

EXPERIMENTS

EXPERIMENTS

47
Experiment: Basic Lab Techniques in Analytical Chemistry Chem251 modified 08/2018

48
Experiment: Basic Lab Techniques in Analytical Chemistry Chem251 modified 08/2018

00 Experiment: Basic Lab Techniques, Compliance of GLP and Calibration of Glassware

OBJECTIVE: In this experiment you will learn the basic techniques when carrying out chemical analysis. You will learn how to use the
analytical balance, calibrate Eppendorf pipettes, read volumetric glassware and calibration of glassware. Finally you will practice taking
meticulous notes on your procedure and observation throughout this exercise.
Equipment Chemicals
Analytical Balance Burets (2) Thermometer KMnO4 solid

100 ml Vol Flask 50-ml Beaker Stirring rod Deionized water

10-mL Vol pipet Slop bucket (400 ml beaker) 10-mL grad cylinder Aluminum slug
250 ml Vol Flask 125-mL Erlenmeyer flask (2) Pipet bulb 5 – pennies in container
Rubber stopper or cork- 400-mL beaker

SAFETY AND DISPOSAL INFORMATION

Dispose of ALL solid permanganate, permanganate solutions, and washes containing permanganate into the proper, labeled
Hazardous Waste Container in the hoods. If you are unsure about the location of the Haz-Waste container, ASK! Never pour
any reagents or chemical down the sink.
Please complete the prelab for the second day which is to generate the tables in your notebook. This lab starts on day2 of the term!!!
Those without a hard copy of this procedure and without a lab notebook will not be allowed to begin the calibration procedures.
Please use care when using the analytical balance. Wipe all moisture left on balance. Before the end of the day, be sure the balance
room is clean and all trash and waste have been disposed. Close the chamber window of your balance before excusing yourself from the
balance room. It is everyone’s responsibility to keep the balance room clean at all times.
You may dispose of water down the drain.
RECORDING DATA: Use only the lab notebook designated for this course otherwise you will lose 10 pts. Start on page 4 or 5
in your lab notebook, saving the first few pages for table of content and miscellaneous information.
If directed by your instructor, you will need to reproduce the data table in the next few pages in your lab notebook. Record all data in
your lab notebook, and DO NOT use pieces of scrap paper while recording your work. If I observed you doing this, you will lose points in
your technique grade. Record your procedure and observations in your notebook (see grading evaluation for this experiment). Remember
for all experiments in this course, you absolutely need to use your Laboratory Notebook. Your instructor will confiscate pieces of
scrap papers, on which you have written data or information, upon discovery. In other words, DO NOT EVER COME UP TO
YOUR INSTRUCTOR WITHOUT YOUR LAB NOTEBOOK TO SHOW DATA OR TO ASK QUESTIONS, you will be marked down
for not keeping with the protocol or for noncompliance of GOOD LAB PRACTICE.
UNKNOWNS: The instructor will provide you the unknowns for this laboratory. If the instructor forgets, ask the instructor for the
assigned unknown number. A numbered aluminum slug in a glass vial will be your designated unknown. You will weigh the aluminum slug to
the precision of the scale. Upon completion of the procedure, place the slug back in the vial and return the unknown back to where
you found it. If you have to repeat the weighing procedure, you will be issued a new unknown number to carry out your analysis.
DISCUSSION: The purpose of this experiment is to introduce you to the tools and techniques necessary for success when carrying out
chemical quantitative analysis. The techniques are considered one at a time, as though they were unit operations. You may well have
performed each of these techniques in previous chemistry labs, or even in undergraduate research, and you may be absolutely certain
you know how to perform these techniques well. This is immaterial, and you’re probably wrong anyway. There’s a wise, old adage: “It isn’t
the things you don’t know that get you into trouble. It’s the things you know for certain that just aren’t true.”
All volumetric ware should be painstakingly free of water breaks before being calibrated. Burets and pipets need not be dry; volumetric
flasks should be thoroughly drained and dried at room temperature. The water used for calibration should be in thermal equilibrium
with its surroundings. This condition is best established by drawing the water well in advance, noting its temperature at frequent
intervals, and waiting until no further changes occur. It is very important that you never assume that your glassware is clean.
Furthermore, do not ask another classmate or instructor if the glassware is clean, you are responsible for your own work not your
classmate or instructor.
The Analytical Chemistry laboratory requires a substantially higher level of precision, accuracy, laboratory technique, and cleanliness
than any other laboratory you have taken. You have to be both meticulous and patient in this course. If you are careless in your work,
analytical chemistry is not for you. Drop this course now.
Much as a golfer studies, practices, and improves individual discrete skills of the game (the grip, the stance, the swing, driving, putting,
etc.) and puts these all together when playing a round of golf, the chemist must study, practice, and improve individual laboratory
techniques such as pipetting, weighing, transferring solids and solutions, and reading a buret to do a complete analysis properly. Do not
be lazy and cut corners. This course is to help you hone your skills when working in a laboratory so take advantage of the experience.
The whole point of this experiment is to learn proper technique for individual skills first, before attempting additional labs. If you
can’t read a buret properly or pipet accurately or reproduce the technique reliably, it is foolish to attempt a complete volumetric
analysis. Therefore, if any parts of this experiment need to be redone to satisfy the various tolerance levels, redo them as soon as
possible, and document the new data set in your lab notebook. If you do not meet tolerance limits after two or three tries, you are
obviously doing something wrong. Ask for assistance from your instructor.

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Experiment: Basic Lab Techniques in Analytical Chemistry Chem251 modified 08/2018

GRADING OF EXPERIMENT #1
This experiment is graded differently from the other labs. Each part in the procedure must be passed within the acceptable tolerance.
Each part is independent of the other. Once one part (parts A, B, C, D and E) is successfully completed, points will be earned for
successful completion. An additional 15 pts will depend on your record keeping techniques and how well you compile your results. To
ensure that these important skills have been mastered in a timely fashion, this experiment MUST be successfully completed and turned
in by deadline as outline in the lab schedule. If not, zero points (0 pts) will be awarded.
There is no “partial credit” on the procedural part of the experiment. You will earn 5pts or 0pts for each technique. After
completion & turning in the write-up for the lab, additional points will be added to the overall score depending on unknown scores
& the write-up.

PART A: USE OF THE ANALYTICAL BALANCE TO CALIBRATE EPPENDOEF PIPPETTES (5 + 5-pts Unknown Aluminum Slug)
Read section 2.6 of the Harris Text (8th edition)
Automatic adjustable micron pipettes have become an indispensable tool in today's biochemistry laboratory. They are highly
advantageous due to their accuracy, ease of use, and wide range of volume deliveries available. You will be using the Eppendorf line of
pipettes in this lab. The identification numbers found on the side, as well as the color on the top button, give the pipette size. The
pipettes provided allow for delivery of 1 - 1000 microliters in the following volume ranges:
Micro Pipette Volume Range
VWR 20 – 200 uL
Fingerpipette II 100 – 1000 uL

Each micro pipette is to be used with a specific disposable tip provided in the plastic racks. These pipettes must never be used
without a tip! The small clear tips are used with the Eppendorf VWR, 20-200 , and the large blue tips with the Eppendorf 1000. Tips
may be used more than once when delivering the same solution, but always replace the tip when changing solutions, when using sterile
solutions, or if it becomes dirty, contaminated, or if liquid droplets seem to be retained along the pipette walls. Tips are not stable for
chloroform or concentrated nitric or sulfuric acid. In most cases tips are best used for aqueous solutions. Calibrating pipettes
frequently is necessary to identify pipettes that are not delivering accurately. Before calibrating the pipettes, practice using the
pipettes and get a feel of the button.

The following is a specific sequence of steps that are followed each time a transfer is desired. This is the “forward mode”.
1. Set appropriate volume on appropriate model. 6. Inspect solution in tip to confirm that no air bubbles are present.
2. Carefully attach appropriate tip to model. Do not press down on 7. Place tip gently against the side of destination container.
tip too hard, but do insure that tip is firmly attached. 8. Push large button to first stop.
3. Press the large button until the first stop. 9. Push large button to second stop.
4. Place the tip in the solution to be transferred. 10. If necessary, dispose of tip by pushing smaller button on the
5. Slowly and smoothly release the large button. back of pipette grip.

These pipettes are very fragile and expensive. You are the primary users of these fine instruments and therefore, it is your
responsibility to maintain the pipettes in fine working condition. You will be held responsible for any damage to your pipettes due to
neglect. In addition to the guidelines already provided, the pipettes should never lay in a horizontal position with a full tip. If you draw
too much liquid then the pipettes become flooded in the inside with the liquid. Make sure you use the correct tips to prevent this.

Calibration is carried out at ambient temperature. In addition, obtain an unknown number from your instructor for an aluminum slug. Do
not use the same unknown as a classmate otherwise you will split the points. Write your unknown number and the mass data in an organize
table in your lab.

You will be given a pipette and also be assigned a balance, be sure to use this same balance for the duration of the course. Write in your
notebook the ID of the balance you are assigned. It is up to you to keep your balance clean at all times. If your balance has been un-
kept, you will be penalized in your lab technique score. It is also important to write notes to yourself on the proper operation of the
scale. Write these notes in your lab notebook
All adjustable pipettes should have their calibration checked periodically. The easiest way to accomplish this task is to pipette an
indicated volume of a solution of known density, weigh the amount transferred, and determine if the measured volume corresponds to
the indicated volume. The density of distilled water at 25°C is 0.997075 g/ml; an Eppendorf 100 pipette set to 055 should deliver 55 µL,
which will weigh 0.0548 g based on the formula: Weight = Density / volume.

In order to establish the accuracy of your pipettes and to test the reproducibility of your pipetting technique, you will pipette ten
aliquots of distilled water from one of your pipettes, carefully recording the cumulative weight after each addition. You will calibrate
each pipette using 2 trials at 1 settings (80%). So, if you are calibrating a 100-1000uL pipette, set the volume to 800uL (.8 mL). If you
have time, also do the same procedure at the 20% volume setting. You will be emailed the calibration technique and the proper technique
or you can download it from the website.

50
Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Procedure, Part A
After your instructor has instructed you on the proper use of the electronic balance and you have become familiar with its use, decide
which pipette to calibrate. Since there is no time to calibrate all your pipette, it is recommended that you calibrate the pipette that is
used most often, the 100 – 1000uL pipette (at 80% capacity).
For this part choose an aluminum slug unknown that is the same as your Eppendorf / Buret number. That is if you have Eppendorf/Buret
#4, your unknown number in the course will also be #4.
1. Go to the analytical balance that has been assigned to you.3 Make sure the balance is level and had been warmed up for at least 30
min. Place a weighing boat on the analytical balance and accurately weigh the empty boat to the full resolution of the balance (0.1mg).
This first procedure will be for setting of 80% volume of your pipette. Now, carefully pipette an aliquot of distilled water into the boat
and record the weight. Repeat this process recording the cumulative weights of ten aliquots. Remove and dry the weighing boat with a
Kim-wipe and repeat the process for the second trial using the same pipette at 80% volume. At the end of the experiment you should
have two sets of ten weights for the pipettes you have selected to calibrate. Be sure that you have recorded your data in your
notebook. Use your thermometer to measure the temperature of the distilled water and use the table of values below to find the
density. If you have time repeat this procedure at 20% volume. You can repeat this for your other pipettes to determine their
accuracy. This is not required.
Table 1. Density of pure water for various temperatures.

Temperature density Temperature density Temperature density

(° C) (g mL )
-1
(° C) (g mL )
-1
(° C) (g mL-1)

16.0 0.99897 21.0 0.99802 26.0 0.99681

16.5 0.99889 21.5 0.99791 26.5 0.99668

17.0 0.99880 22.0 0.99780 27.0 0.99654

17.5 0.99871 22.5 0.99768 27.5 0.99640

18.0 0.99862 23.0 0.99757 28.0 0.99626

18.5 0.99853 23.5 0.99745 28.5 0.99612

19.0 0.99843 24.0 0.99732 29.0 0.99597

19.5 0.99833 24.5 0.99720 29.5 0.99582

20.0 0.99823 25.0 0.99707 30.0 0.99567

20.5 0.99812 25.5 0.99694

2. Take the vial assigned to you containing the aluminum slug. Be sure that you have a unique unknown number from your classmate. Also
remember that if you do not record your unknown number in your notebook, you will not receive any credit. Record condition of the
unknown, weigh the unknown aluminum slug and record its mass.

Return the Al slug to their appropriate vial as soon as you have successfully completed the procedure and return the vial to your
instructor.

3. Using Excel, type in each of the datasets as (cumulative weight - weight of empty boat) versus (total volume added). Plot each dataset
(linear option) and fit each plot with a linear regression. Record the slope of the plot, the correlation coefficient and obtain an error
estimate for each dataset. Printouts of these plots should be included in your lab notebook. Share this information with your lab partner

4. For all two datasets, convert the cumulative weights into a table of weights per aliquot. Enter these data into the spreadsheet and
obtain appropriate statistics for each set. Divide the mean weights by the density (corrected for temperature) to obtain the mean
volumes delivered. Calculate the percent error for each of the two volume pipettes. Share this data with your lab partner.

In your laboratory notebook you should include the plots prepared above and a table reporting slopes, and the mean, median and standard
deviation for each dataset, as determined from your analysis. A second section of the table should report these same data as obtained
by your lab partner. You should also comment on the accuracy and the reproducibility of your pipetting, a comparison of your error and
your partner's and the correlation between the volumes indicated on the pipettes and the actual volumes delivered. Please note that
your notebook will be scrutinized by your instructor and you should utilize this opportunity to practice writing for future and more
involved laboratory reports.

NOTE: NEVER transfer chemicals inside an analytical balance. In this experiment, however, it is okay to pipette water to a
weighing boat. If you spill any liquid on the balance, soak up the residual liquid immediately with Kim-wipes and contact your
instructor.

51
Quantitative Analytical Chemistry, Lab Manual Modified 8/18

PART B: QUANTITATIVE TRANSFERS (5-pts)

This procedure is designed to provide experience for the correct use of the volumetric flask. Record your observations in your labbook.
1. Tap a very small amount of potassium permanganate, KMnO4, from the stock bottle onto a piece of folded glassine paper or into a
small clean beaker or a plastic weighing boat. (Note: Returning chemicals back into stock bottles should never occur as this may
contaminate the entire bottle. Avoid putting a spatula into a stock bottle. Tap out a small amount if at all possible.)
2. Tare a clean, dry 50-mL beaker on an electric top-loading balance that is found at the front of each lab counter. Use this scale and
not the analytical balance for this procedure. (Note, for weighing that do not require precision to the tenth of milligram, use this top-
loading balance.) Add about 0.2 g of KMnO4 to the beaker, this will be used to prepare a 100-mL stock solution.

3. Dissolve the potassium permanganate in about 20 mL of distilled water, stirring gently to avoid loss. This is
nearly a saturated solution, and some care is required to dissolve the crystals completely.
4. Quantitatively transfer the solution into a 100-mL volumetric flask using a small funnel. To prevent the
solution from running down the outside of the beaker, pour the solution down the stirring rod, and then touch
the rod to the spout of the beaker to remove the last drop. If needed, ask your instructor to show you how to
do this. Add more water to the beaker, stir, and repeat the procedure.
Record the amount of washing and the number of times required to quantitatively transfer the permanganate from
the beaker to the flask. Finally, rinse the last portions of solution from the stirring rod into the volumetric flask
with a stream of water from the wash bottle. Rinse the funnel and remove it. Carefully dilute the solution in the
flask until the bottom of the meniscus is even with the graduation mark.
5. Stopper, invert, and shake the flask. Return it to the upright position, and allow the air bubble to return all
the way to the top of the neck. Repeat until the solution is completely homogeneous; a minimum of 10
inversions and shakings will be required. Save this solution for Part C.

PART C: TAKING AN ALIQUOT (5-pts)

Whenever a buret or pipet is used to deliver a measured volume of solution, the liquid it contains before a measurement must have the
same composition as the solution to be dispensed. The procedure referred to in this section is called “conditioning” your glassware. The
following operations are designed to illustrate the minimum effort needed to ensure this.
NOTE: During this part, collect all the permanganate solutions and rinse waste in a large beaker (“slop bucket”). At the end, all the
permanganate is to be disposed of in the proper, labeled waste container. No permanganate should go down the drains.
1. Before beginning this section, make sure you know how to use the Brinkman
pipet bulb mechanism in your lab drawer. Your instructor will illustrate how to
use this or show you a video on the proper use. [Never draw so much solution
that it fills the suction mechanism. If you do this you will ruin the suction
mechanism and this will reflect in your lab technique score.] Fill a pipet with
the solution of potassium permanganate and let it drain completely into a waste
beaker. Wait 20-30 seconds, then touch the tip of the pipet to the side of the
beaker. Draw a small amount of distilled water from a 50-mL beaker into the
pipet, rinse, and discard the rinse solution. Do not fill the pipet completely;
this is wasteful, time-consuming, and inefficient. Just draw in a small amount,
tilt the pipet horizontally, and turn it to rinse the sides. Determine the
minimum number of such rinsing required to completely remove the
permanganate color from the pipet. [Hint: Look at the liquid that collects in
the tip of the pipet against a white background to see if there is any
coloration.] If your technique is efficient, three rinsing should suffice. (Note,
if you are not comfortable with the Brinkman pipet bulb, ask for an alternate.)
2. Fill the pipet again with permanganate and proceed as before. This time To use the Brinkman Pipet Bulb.
determine the minimum volume of rinse water required to remove the color by 1. Squeeze air out of bulb to create a partial vacuum.
2. Insert a pipet into the pipet receptacle.
collecting the rinsing in a small graduated cylinder (less than 5 mL of rinse
3. Place tip of pipet well into the liquid.
water is enough with efficient technique). Check the pipet tip for coloration.
4. Push lever up to draw fluid above desired calibration
**3. Upon the discretion from your instructor, you may be asked to show off line. DO NOT DRAW FLUID INTO THE BULB!.
the following aliquot technique. Condition a 10-mL pipet three times with the 5. Press level down to deliver fluid to new container.
solution of potassium permanganate you prepared (above). Pipet 10 mL of the 6. Press bulb to blow out last of the liquid from the pipet.
For more details go to:
permanganate solution (see section B, step 2) into a 250-mL volumetric flask.
http://abacus.bates.edu/~ganderso/biology/resources/serological_p
Carefully dilute the solution to volume, try to minimize the mixing of the 10-mL ipet.html

KMnO4 solution with water in the dilution process. Now, mix the solution by repeatedly inverting and shaking the flask. (Note the effort
required to disperse the permanganate color uniformly through the solution.) Rinse the pipet with the solution in the volumetric flask.
Pipet a 10-mL aliquot of the solution into a 125mL Erlenmeyer flask. Remember to condition the pipet before drawing the 10-mL aliquot
** You may be picked at random to demonstrate your technique.
4. (Optional) If your lab technique is satisfactory, ask your instructor to initial your report to indicate passing this part of the lab.

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

PART D: CALIBRATION OF A GRADUATED PIPET (5-pts)

Read section 2.6 of the Harris Text (8th edition)
The calibration of an analytical transfer pipet is a relatively straightforward procedure. The proper technique is readily learned with
practice, care, and attention to detail. Note that this is a manual technique. It must be learned; it does not magically appear on the first
try, not unlike learning to hit a golf ball. With some practice, however, you ought to be able to handle a pipet about as well as who
routinely works in an analytical lab. With the exception of a simple weighing, this experiment is capable of being the most accurate and
precise set of measurements you’re likely to ever perform in a lab course.

1. Obtain the following equipment: Pipet bulb (Brinkman pipet bulb); 125-mL Erlenmeyer flask with a dry cork or rubber stopper; 400-mL
beaker of distilled water equilibrated to room temperature; and a thermometer.

2. Clean a 10-mL pipet, and be sure that your pipet is ultra clean. Cleaning is usually accomplished by drawing some warm soapy water into
the pipet bulb, wetting the sides, and “shaking the soap” inside the pipet. If that doesn’t work, soak the entire pipet in soapy water
overnight or longer. You must clean pipets, burets, and other pieces of volumetric glassware, so that no droplets of reagent remain on
the internal surfaces when they are drained; there should be no water break. This is very important for accurate and reproducible
results. If reagent gets “hung up” inside a pipet, you obviously cannot deliver the nominally stated volume. You should have already
cleaned your pipet properly during the check-in period.

3. Using the analytical balance, weigh the flask and stopper and record the mass to the nearest 0.1 mg. Do not touch the flask with your
fingers after this weighing. Use tongs or wear gloves.

4. Read and record the temperature of the water.

5. Pipet 10.00 mL of the distilled water into the flask using the technique described above. Re-stopper the flask, weigh it, and record
the mass of the stoppered flask plus the water.

6. Add a second pipet of water to the flask, without pouring out the 1st aliquot, removing the stopper just before the addition. Re-
stopper, weigh, and record the weight. Repeat the entire procedure for a minimum of four readings that agree to within a total range of
less than about 0.02 g for all the readings. [If you have what you consider 3 “good” replicates and one that seems “bad”, try the Q-test
to see if the outlying value can be rejected.] If your values seem very non-reproducible, throw out all your data and do another full set
of 4 minimum, paying closer attention to what you’re doing. If these still do not reproduce well, there is something clearly wrong with
your technique. Seek assistance from your instructor. Have your instructor look over your measurements in the data sheet and initial it
upon satisfactory completion of this section.

7. Correct the apparent masses of the aliquots for the buoyancy effect of atmospheric air to get the true masses as described below.
Then calculate the true volume of the pipet using the density of water at the temperature(s) of each aliquot.

8. Report the average “true volume” of your pipet and the associated standard deviation of your values.

Correction for Buoyancy3

A buoyancy error will affect data if the density of the object being weighed differs significantly from that of the standard weights
(inside the balance for an electric balance). This error is due to the difference in the buoyant force exerted by the medium (air) on the
object weighed and on the weights themselves. The correction is made using:

mcorrected = mobserved + mobserved [(dair/dobject) – (dair/dweights)]

where m is the mass in grams of the corrected and initially observed values of the object weighed (in this case, distilled water, see table
below), and d is the density in g/cm3 of air, the object, and the weights. For all but the most exacting work, this correction is negligible
for solids and liquids having a density of 2 g/ cm3 or greater. Correction for buoyancy is required only for measurements that require
the highest accuracy, for gases, or for low-density solids and liquids. The density of the weights used in electronic single-pan balances
ranges from 7.8 to 8.4 g/cm3, depending on the composition of the weights. Using d = 8 g/cm3 is adequate for most purposes. The
weights

dair = 0.0012 g/ cm3 at room temperature and pressure.

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PART E: BURET ASSIGNMENT: READING OF BURET (5-pts)

Read section 2.4 of the Harris Text (8th edition)

1. You will be issue 2 burets for this course. Be sure to label your burets because these will be stored under hood #1 since burets cannot
fit in your drawer. You can use a wax pencil or a label tapes to do this. Burets are normally stored upside down so that the inside
surface of the part of the section where you will take your reading will remain wetted and drain well. It is also recommended that upon
storing the buret, you place parafilm on the tips of the buret so that you minimize contamination to the interior of the buret. Use the
buret stand to keep the buret vertical. Puncture a pin size hole at the ends so as to have any residual water drain out of the buret.

2. Invert the buret and tap the section lightly to remove any solvent that might remain in the sealed tip and let it drain for at least 20-
30 sec. Use a buret reading card to estimate the readings to the nearest 0.01 mL. A buret card is easily made by making a very heavy,
black horizontal rectangle in the center of a 3 x 5” file card.

3. Over-fill the buret with distilled water. You can over-fill the buret by adding distilled water past the 0.0-mL mark. Make sure that
there are no air bubbles trapped in the tip. If so, rapidly open valve, “full throttle” until the bubbles are flushed out. If this does not
work, sometimes a quick vertical jerk will loosen any residue lodged at the tip of the buret. Refill the buret if the water level falls below
the 0.0-mL mark.

4. Drain the buret down to someplace between 0 and 1 mL. Do not try to bring the buret to exactly 0.00 mL, as this is a waste of time.
The “zero” reading on all but an automatic buret is always some finite non-zero reading.

5. Wait at least 20-30 seconds before taking the initial or “zero” reading. Why? Take the initial or “zero” reading and the other buret
reading using a buret reading card.

6. Now let about 5 mL run into a 125-mL Erlenmeyer flask. Wait at least 30 seconds and take the “final reading”. (The amount of solution
in the Erlenmeyer flask is equal to the final reading minus the “zero” reading.) Write down the final reading on the data sheet provided,
the time you waited before reading the buret, and then ask your instructor to take the final reading. Compare the two readings. They
should agree within 0.01 mL. Do they? Notice that the final digit in the buret reading is the estimation of the distance between two
marks on the buret. The instructor will initial your datasheet upon satisfactory completion of this part.

7. Refill the buret, and take a new zero reading. Now add 30 drops to the Erlenmeyer flask, and take the final reading. Calculate the
average volume of one drop, then repeat this except with 40 drops and calculate the average volume of a drop. Record these results and
compare them. Now, practice adding “half-drops” to the flask. Calculate the average volume of your “half-drops”. In several titration
experiments, you will want to try to get half-drop end points for good precision.

PART F: CALIBRATION OF BURET (10-pts) (Taken from C. Harrison, SDSU)

You may calibrate just one or both of your buret. If you decide to do only one, then remember that when doing your titrations, you want
to use the calibrated buret for precise measurements.

There are inherent errors in the volumes indicated in the barrel of a buret, which will cause your results to deviate. For this reason you
will need to calibrate your burets. Because the burets do not drain in its entirety during a single titration, calibration must be done in 10
ML increments.

1. For this calibration you will need a stopper flask of 50 mL or greater (but not to exceed the balance weight limits), DI water, a
thermometer and your burets. Before you begin, be sure your burets are clean and the stopcocks are functioning properly.

2. Fill a clean, large (~400 mL), beaker with DI water, insert a thermometer and give the water time to come to equilibrium with the
room temperature.

3. Prepare a table in your lab notebook, similar to the ones on the following page. You will need to perform the calibration process at
least twice to obtain matched, replicate data for the calibration.

4. Record the temperature of the DI water. Record the mass of the flask and stopper.

5. Fill the buret with enough of the DI water so that the meniscus is between the 0.01 and 0.30 mL lines; ensure that there are no air
bubbles in the tip of the buret. Do not attempt to fill the buret to 0.00 mL, this is pointless, time consuming and does not provide any
benefit to an analysis.

6. Record the initial volume of the buret. Next titrate water into the flask until approximately 10 mL have been delivered.

7. Stopper the flask as soon as you are done delivering the water. Record the new volume on the buret and the new mass for the
stoppered flask.

8. Repeat the process for each 10 mL increment of the buret - do not bring the level of the water below the 50.00 mL line as you cannot
measure the volume beyond that point. The whole process will need to be repeated a second time in order to confirm the results of the
first calibration. In some cases, multiple calibration attempts will be needed to ensure that the calibration is accurate.

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Calculations: The calculations of “true weight” and “true volume” are obtained using the buoyancy correction and density calculation as
performed for the pipette calibration (page 16). All other calculations are direct subtraction or additions. The cumulative correction is
the sum of the correction values of each or the preceding intervals

Error Check

To check for any arithmetical errors in the table a simple equation can be used. The letters in the equation below are to be replaced with
the values in the table cells with the corresponding letter (e.g. C = -0.01)

A - B + C = D - E + 5(G-F)

The difference in value on both sides of the above equation should be within 0.02 of each other. If the difference is greater than 0.02
there has been a calculation error in the table and it must be corrected.

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Calibration Check

In order for a calibration to be accurate it must be replicable. Therefore you will do two (or more) calibration tables for your buret.
Once the calculations for the table are complete and each table has passed the error check (above) the data can be compared to see if
the calibration was reproducible.

The tables on the previous page each had a set of cells that were shaded in light grey, the values in these cells (copied below) need to be
compared between tables. To compare the values, subtract the value segment correction of trial 2 from that of trial 1. The errors in the
individual segment corrections must be less than or equal to 0.02 mL. For the total cumulative correction, the error can be no greater
than 0.04 mL. In the example below, the calibration failed because the error in the corrections for the 20 - 30 mL segments differed by
more than 0.02 mL. Thus, a third calibration must be done.

Calibrated Volume

Once you have completed the calibration of the buret you will need to generate a calibration graph so that you can make use of the
information that you have collected. Use the grids in your lab manual in order to has been included at the front of this lab manual for
you to use in making your calibration graph. The graph will be a simple tool that you can use to correct for errors in the measured versus
actual delivered volume from your buret.

To construct the graph, determine the average correct for each 10 mL segment of your buret, based on the two replicate calibrations.
Once you know the average correction volume, plot this value against the nominal volume at the end of each segment (e.g. 10, 20, 30 mL).
The graph below is a calibration graph based on the data above (presume that the correction for 20 - 30 mL in trial 2 had an error of
0.00 mL).

You will use the graph to determine the proper volumes delivered from your buret. Simply record the value read from your buret, then
apply the appropriate correction to your titration calculation

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Example:

Calculations and Post-Lab Write-up (10 pts)

An excel spreadsheet may be available to you so that you can take the measurements from this lab and automatically perform needed
calculations. If one is available, use excel to perform all pertinent calculations. If an excel template is not available, you should
generate one. You can use the structure of the datasheet here to give you a sense of how to organize your data in the excel
spreadsheet. You will be asked to generate spreadsheets through out this course so you will develop skills on producing data sheet that
can be easily analyzed. While using excel to present your data and to perform repetitive calculations is convenient, you must however
show a sample manually calculation in your lab notebook and especially when the procedure instructs you to do so. You need not worry
about a sample calculations for some statistical calculations however like the standard deviation, simply state that the results was
determined by an excel function. If your class is using a virtual “cloud” drive to store data, i.e., Google Drive or DropBox, you should
store the result in this experiment in the appropriate folder in the virtual drive. If you don’t know how to do this, ask your instructor
for help.

Summarize each of the part of this experiment and discussed how each of these parts are important in Analytical Chemistry and what
you learned in the procedural process. Keep your total summary to one type written page.

REFERENCE

1. D. A. Skoog, D. M. West, F. J. Holler, and S. R. Crouch, Analytical Chemistry: An Introduction, 7th ed. Chapter 2, pp. 21-59.
2. Mark J. Rudin, William H. Hohnson, UNLV, Dept of Health and Physics
3. Topic on Analytical Balance and Buoyancy correction, Section 2.3 of the Harris Text (8th edition)

4. Topic on Burets, Section 2.4 of the Harris Text (8th edition)

5. Topic on Pipets an Syringe, Section 2.6 of the Harris Text (8th edition)

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00 Basic Lab Techniques in Analytical Chemistry; Calibration of Glassware

Reproduce this table in your lab notebook

____ / ___ Score Last Name ________________________First____________________ Date _____

Datasheet.

Part A(i) Use of Analytical Balance and Pipette Calibration

Part A (i) Adding water from pipette in Analytical Balance

Trial 1 Trial 2 Trial 1 Trial 2

Pipette ID -Total Running Mass -Total Running Mass Pipette ID -Total Running Mass -Total Running Mass

_________ Mass of each drop Mass of each drop _________ Mass of each drop Mass of each drop

Readings of Balance after tare Reading of Balance after tare

#1 #1

#2 #2

#3 #3

#4 #4

#5 #5

#6 #6

#7 #7

#8 #8

#9 #9

#10 #10

Total mass Total mass

for drops for drops
1 - 10 1 - 10

Statistical Analysis: Pipette #1 Pipette #2

Average Mass of drops (g)

Standard deviation (s)

Relative standard deviation or coefficient of variation (CV)

A(iii): Weighing unknown mass of Aluminum

Al Slug Unknown # Condition Mass (g)

Instructor's initial: Initials _______

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Part B Qualitative Transfer

Part B (i) Preparing 100-mL KMnO4 solution

Observation Data

Step 2 Mass KMnO4

Step 4 Amount of washing to transfer KMnO4

from beaker to flask (mL)

Part C Taking an Aliquot

Part C (i) Using a pipet and suction mechanism to prepare a solution.

Observations Data

Step 1 Minimum number of rinse to completely remove KMnO4 color from pipet

Step 2 Minimum volume of rinse water required to remove KMnO4 color from pipet

Step 3a: Preparing 250 mL stock solution,

Step 3b: Aliquot transfer of 10-mL pipet to 125mL Erlenmeyer flask,

Instructor's initial Initials ___________

Part D Calibration of a Pipet

Part D Weighing volumes of water

Data

Step 2, clean pipet

Step 3: Mass of 125mL Erlenmeyer flask and stopper
Step 4: Temperature of water

Apparent Corrected
Mass (g) Mass Mass
Step 5: Mass of flask after transfer 10mL DI water (g)
Step 6a: Mass of flask after 2nd transfer 10mL DI water (g)

Step 6b: Mass of flask after 3rd transfer 10mL DI water (g)
Step 6c: Mass of flask after 4th transfer 10mL DI water (g)

Average True Volume and standard deviation

Instructor's initial Initials ___________

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Part E Use of Buret

Part E (vii) Reading a buret

5-mL aliquot reading Vi Time Vf VTotal

Observations:

Instructor’s reading Initial _______ ______

Part E (viii) Counting Drops

Avg Vol *

Determining volume in a drop and half-a-drop Vi drops Vf VTotal per drop

Observations (1 drop procedure, 30 total drops):

* Show calculations here

Observations (1 drop procedure, 40 total drops):

* Show calculations here

Observations (1/2 drop procedure, 30 total half-drops):

* Show calculations here

Observations (1/2 drop procedure, 40 total half-drops):

* Show calculations here

Observations (mulligan):

* Show calculations here

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00 Experiment: Basic Lab Techniques and Compliance of GLP Analytical Chemistry 251
# CRITERIA (Tentative point distribution) pts

A Use of the Analytical Balance (5 + 5)

i. Record Keeping of Pipet Calibrations:
• Notes on using a balance. 5
• Record keeping for pipet calibration. Observation in complete sentences
• Precision in measuring mass
ii. Mass of Unknown, Aluminum Slug
• Unknown number data 5
• Unknown mass __________ (True) / ____________ (Recorded)
• Notebook initial by instructor.
B Quantitative Transfer (5)
i. Recording data and technique in quantitative transfer
• Notes on preparing KMnO4 solution. 5

• Notes on number of washing to quantitatively transfer from beaker to flask

C Taking an Aliquot (5 + 5)
i. Using the Brinkman pipet
• Notes on using the Brinkman pipet and making the transfer 5
• Technique on using the Brinkman pipet (instructor's notes)
• Notes on number of rinse required to remove permanganate purple color
ii. Demonstration to instructor 5
• Grade on technique for conditioning and preparing KMnO4 solution demo to instructor.
• Notebook initial by instructor.
D Calibration of Pipet (5 + 5)
i. Preparing pipet
• Notes preparing pipet 5
• Mass of flask, stopper and water. Precision and accuracy
ii. Buoyancy correction procedure and calculations
• Analysis of 3 good weighing. 5
• Buoyancy correction calculation.
• Average "True volume" of pipet.
E Buret Assignment and Proper Reading of your Buret (5 + 5)
i. Caring and labeling buret 5
• Notes on caring and storing buret
ii. Conditioning and preparing buret
• Notes on preparing and conditioning buret
• Notes on using the buret card to read meniscus of buret.
iii Reading buret to correct precision 5
• Instructor reading confirmation. Reading should be with in +/- 0.02 mL and correct precision
iv. Practice half drop technique
• Notes on technique of half-drop techniques.
Lab Techniques / Record keeping / Excel Workup (5)
• Following directions of lab and course.
• Precision of work, sound statistical analysis, conclusion of results 5
• Upkeep of notebook, notebook preparation and using proper notebook as instructed by syllabus
• Working diligently and independently without excessive guidance by others.

Instructor's Comment

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1
01 Experiment. Molar Mass of an Unknown Sulfate Salt by Gravimetric Techniques
This lab is to reacquaint you with some basic laboratory techniques and serves as a warm-up to the experiments in this course.

Lab Overview: The amount of sulfate ions in a product will be determined by precipitation of its salt as a secondary BaSO4 product.

Stoichiometry calculations will be used to identity of the molar mass of the sulfate salt. A strategy to obtain the best results, is to

isolate BaSO4 as large crystals. Two methods will be used to dry the crystals, one is by using glass frit funnel filtration technique and

the second is to collect the precipitate using ashless filter paper and then igniting the precipitate to recover the BaSO4. The two

results will be compared to determine if one method is more effective over the other.
1.
Read Chapter 27 in Harris (9th Ed) or Chapter 26 (8th Ed), before beginning this experiment.

Reagents and Equipment: The lab techs will prepare the following solution for the class-
Crucible and Cover Ashless filter paper (110 mm diameter) 0.1 M BaCl2 solution
Glass frit funnel Alkali or alkaline salt unknown 6 M HCl solution
25-mL Vol Pipet

Safety: Be careful when handling 6 M HCl. If any HCl comes in contact with your skin or eyes you should immediately wash with water

for several minutes. You should be wearing your lab coat, gloves and your goggles at all times. Make sure to allow ample time for the

crucible to cool after it has been heated.

Gravimetric analysis is a quantitative method for accurately determining the amount of a substance by selective precipitation of the

substance from an aqueous solution. The precipitate is separated from the remaining aqueous solution by filtration and is then weighed.

Assuming that the chemical formula for the precipitate is known and that the precipitation reaction is stoichiometric (goes to

completion) the mass of the substance in the original sample can be determined.

In this experiment, you will determine the percentage (by mass) of sulfate in an unknown sulfate salt by gravimetric analysis. First you

will dissolve a measured mass of the unknown salt in water. Next you will add a measured excess amount of aqueous barium chloride to

the aqueous solution of the unknown salt. This will result in the precipitation of the sulfate as barium sulfate. The filtrate will be

collected for analysis in a later experiment.

BaCl2 (aq) + M2SO4 (aq) → _BaSO4 (s) + 2 MCl (aq) (assuming +1 cation)

BaCl2 (aq) + MSO4 (aq) → _BaSO4 (s) + MCl2 (aq) (assuming +2 cation)

The number of moles of sulfate can be determined from the mass of the barium sulfate. Since barium chloride is added in excess, and

since the precipitation reaction is assumed to go to completion, the number of moles of sulfate recovered in the precipitate can be

assumed to be equal to the number of moles of sulfate in the original sample allowing for the calculation of the percentage by mass of

sulfate in the original sample.

For best results the BaSO4 crystals should be as large as possible. This facilitates filtration and washing of the crystals and the

decreased surface area minimizes the amount of impurities adsorbed onto the crystals. Generally, the largest crystals are obtained when

the rate of precipitation is as low as possible. The rate of precipitation is minimized by slowly adding the BaCl2 solution to the aqueous

mixture containing the unknown salt while continuously stirring the mixture. The rate of precipitation can be slowed down still farther by

slightly increasing the solubility of the BaSO4 (remember that a substance that is said to be insoluble is in fact very slightly soluble).

The increase in solubility is achieved by lowering the pH with 6M HCl and by increasing the temperature. It has been shown that the

resulting decrease in the yield of the BaSO4 is insignificant under these conditions.

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Procedure
Work with another partner with one using the sintered-glass funnel technique and the other using ashless paper combustion procedure.
Each will work on the same unknown and work independent of each other except to report results. Use deionized water in all the
procedures describe here. Use chilled deionized water when washing the BaSO4 precipitate in step 5 below. At a minimum, you and your
partner should do three trials each.

1. Measure and record (nearest 0.0001 g) the mass of a clean, dry 250-mL beaker using the analytical balance. Add between 0.30 g and
0.35 g of your unknown sample to the 250-mL beaker and record (nearest 0.0001 g) the mass of the beaker plus sample.

2. Add 50 mL deionized water to the sample in the beaker. Next add 20 drops of 6 M HCl to the beaker. Stir the contents of the beaker
until the sample has entirely dissolved. Leave the stirring rod in the beaker.

3. Measure 25 mL of 0.1xx M BaCl2 solution using a volumetric pipet to a 50-mL Beaker. The beaker should be clean and rinsed with

deionized water but need not be dry.

4. Heat the solution containing the sample in the 250-mL beaker until it is nearly (but not quite) boiling. Turn the burner off and slowly
pour small portions of the BaCl2 solution into the 250-mL beaker containing the sample. This step should take at least 3 minutes

otherwise the BaCl2 is being added to rapidly. Stir the contents of the beaker as you add the BaCl2 solution. You should observe the

formation of the white BaSO4 precipitate. Be sure to use all the BaCl2 solution since the unreacted barium ions will be analyze in

experiment 2. Use the wash bottle to rinse the BaCl2 solution in the 50-mL beaker and pour this solution in to the 250-mL beaker
containing the barium sulfate precipitate. Try to use a minimum amount of water in this step however.

5. Rinse any precipitate that remains on the stirring rod with cold deionized water into the solution with a small amount of deionized
water. Allow the precipitate to settle in the beaker in a cold-water bath for about 20 minutes.

a) Procedure for ashless filter paper isolation:

6a. For the lab partner using the ashless paper procedure, prepare your crucible as follows: While the precipitate settles prepare your
crucible by heating it (with the cover on) in the hottest part of the Bunsen burner flame for about 2 minutes. After the crucible has
cooled for 10-15 minutes, place the crucible in the dessicator tray for an additional 15-20 min. When the crucible is at room
temperature, use the analytical balance to record the mass of the crucible and the cover to the nearest 0.1 mg or 0.0001 g. Repeat
the procedure, burning crucible with hot flame, then cooling in dessicator until successive weighing agrees to within 0.5 mg (0.0005
g). If you cannot get with in 0.5 mg after four cycles, then proceed if you are within 1-mg. You will be deducted a few points for
your technique but at least you can proceed on with the experiment. The number of significant figures of your mass should be
consistent with the precision of the balance you are using. Write in your data table the difference in mass between consecutive
weighing.

7a Set up the gravimetric filtration by obtaining a piece of ashless filter paper and fold it into quarters. Open the folded paper into a
cone, place it into a funnel and wet the filter paper with cold deionized water so that it adheres to the funnel. Place a clean 500-ml
Erlenmeyer flask under the funnel to collect the filtrate.

8a After 20 minutes has passed slowly pour the mixture containing the BaSO4

precipitate down your stirring rod into the funnel. Be careful that the level of
liquid in the funnel is never more than three-fourths of the way to the top of the
filter paper. When the transfer is complete use your wash bottle (filled with
chilled deionized water) to rinse the residual precipitate from the beaker and the
stirring rod into the funnel.

9a. Take care to collect all the filtrate in each of your filtration process. The
filtrate contains the unreacted excess barium ions that didn’t form BaSO4. The
barium will be analyzed via EDTA titration in the next experiment. Be sure to save
the filtrate in separate containers and label each filtrate so the trial number is
known.

10a After all the liquid has drained from the funnel very carefully press the top edges of the filter paper together, and fold the filter
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paper into a compact package that will fit into the crucible. In order to avoid tearing the filter paper it is important that you do not
use too much force. Place the folded filter paper into the crucible.

11a Set up your ring stand in the fume hood and support the crucible in a clay triangle that is attached to
your ring stand. Gently heat the crucible without the cover to remove the water. After several
minutes when you are sure the paper is dry, heat the crucible more vigorously so that the filter paper
begins to char (turning from white, to brown, to black) but not so vigorously that the filter paper
bursts into flame. If the filter paper bursts into flame you should smother it with your crucible cover
and lessen the amount of heat. Continue to heat moderately until all of the filter paper has turned black.

12a Once all the filter paper has turned black heat the crucible vigorously with the cover off in the hottest part of the Bunsen burner
flame so that the bottom of the crucible is red hot. The charred filter paper (carbon) will gradually combust and be converted into
CO2 gas. When the filter paper is entirely combusted only the white BaSO4 should remain in the crucible, see insert figure. The

crucible should be heated vigorously until there is no charred filter paper remaining.

13a Allow the crucible to cool for about 15 minutes. When the crucible has cooled to room temperature, place in the dessicator tray to
cool for an additional 15 minutes. When the crucible is at room temperature, record the mass of the crucible, the cover and its
contents to the nearest 0.001g on the analytical balance. Repeat the heating of the precipitate and cooling cycle until successive mass
are within 0.5 mg. If after four cycles, you are not to achieve this, then stop when your mass is within 1 mg between successive
weighing.

14a Store the product in the crucible, the BaSO4 precipitate in another container. The barium content will be analyzed in a future
experiment using the ICP-AAS instrument.

b) Procedure for sintered-glass funnels isolation:

6b. For the lab partner using the sintered-glass funnels prepare your funnels as follow: While the precipitate settles, clean a three
medium-porosity, sintered-glass funnels. Prepare about 50 ml of 1:1 HCl by adding 25 ml of concentrated (12M) HCl to 25 ml of
deionized water. (ALWAYS ADD ACID TO WATER). Rinse the medium-porosity, sintered-glass funnel with a total of 10-15 ml of 1:1
HCl, drawing small volume of the acid through the funnel by suction. Discard the HCl rinses in the collection flask to the appropriate
waste container. Rinse the funnel at least three times with deionized water, drawing a reasonable amount of deionized water through
the funnel. Slowly break the suction of the filtering flask. Discard the water rinses in the filter flask. Next, wash each funnel one at
a time, with acetone from an acetone-washing bottle. Rinse the funnel several times with a stream of acetone and draw air through
the funnel for about five minutes.

7b. Dry the sintered-glass funnels by placing in a large enough beaker to hold the funnels and then placing in an oven to dry for 1–2 hr at
105°C in an oven. Cool the sintered-glass funnels in a desiccator for 30 min. and weigh. Repeat the procedure with 30-min heating
periods until successive mass readings agrees to within 0.3-0.5 mg (0.0005 g). If you cannot get with in 0.5 mg after four cycles,
then proceed if you are within 1-mg. You will be deducted a few points for your technique but at least you can proceed on with the
experiment. Use a paper towel or tongs, not your fingers, to handle the funnels. Alternatively, a 900-W kitchen microwave oven dries
the sintered-glass funnels to constant mass in two heating periods of 4 min and 2 min (with 15 min allowed for cool down after each
cycle). You will need to experiment with your oven to find appropriate heating times. The number of significant figures of your mass
should be consistent with the precision of the balance you are using. Your data table should record the difference in mass between
consecutive weighing.

8b Set up for suction filtration using two side-arm Erlenmeyer flasks, see figure. Be sure the primary Erlenmeyer flask is clean of any
residue since the filtrate will need to be collected. Take care to collect all the filtrate in each of your filtration process. The
filtrate contains the unreacted excess barium ions that didn’t form BaSO4. The barium will be analyzed via EDTA titration in the
next experiment.

9b Begin by filtering each solution through these weighed sintered-glass funnels using
vacuum filtration. Next add ~3 mL of ice-cold water to the beaker, and use a
rubber policeman to help transfer the remaining solid to the funnel. Repeat this

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

procedure with small portions of ice-cold water until all of the precipitate has been
transferred to the funnel. Finally, use two 10-mL portions of ice-cold water to
rinse each beaker, and pour the washings over the precipitate. Save each of the
filtrate in your three trials in different containers.

10b Dry the precipitate by aspirator suction for 1 min, then in an oven at 105°C for 1–2
hr. Bring each filter to constant mass. The product is somewhat hygroscopic, so
only one filter at a time should be removed from the desiccator. Weighing should
be done as quickly as possible. Alternatively, the precipitate can be dried in a
microwave oven once for 4 min, followed by several 2-min periods, with cooling for
15 min before weighing.

11b Upon completion of the experiment, discard the solid precipitate in a chemical clean container. The barium content can also be
analyzed in a future experiment.

12b Wash out the sintered glass funnels with 1:1 HCl solution as done at the beginning of this procedure, 6b.

For more information on technique used in the lab go to the following links:

http://zimmer.csufresno.edu/~davidz/Chem105/DandW/DryW2.html
http://abacus.bates.edu/~ganderso/biology/resources/serological_pipet.html
http://www.youtube.com/watch?v=otye_rFaRlc
http://www.youtube.com/watch?v=x7Nl4el9nrs&feature=relmfu
https://youtu.be/d3EKBT8Fg9A

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Calculations:

Moles of Analysis
A. Moles of sulfate in BaSO4
1 mol BaSO 4 1 mol SO2-4
Moles SO2-4 = mass ppt (g) • •
__ g BaSO 4 1 mol BaSO 4
!##"## $
molar mass BaSO
4

B. Molar mass of unknown sulfate salt:

C. Identity of metal in unknown sulfate salt.

Mass of cation metal in sulfate salt = molar mass sulfate salt - molar mass sulfate = atomic weight of metal (g/mol)
* if the metal is alkali, then divide atomic weight of metal by 2.

D. Report the standard deviation, the relative standard deviation (% RSD) or the coefficient of variation (CV) (Use Excel)
See below see calculations for these statistical parameters.

Next carry out a Comparison of Means with Student’s t.

Decide which case (page 72, Harris, 9th edition) you should use to compare your results with your partner
Carry out the analysis and report your results as shown in the sample data page.

Statistical Analysis:
i) Standard Deviation:
For a population, the measure of the In the real world, it is rare to have a large number of measured value to
absolute precision is the standard work with. It is much more common to have 3-5 values. Moreover, for
deviation. This is found by the equation: unknown samples the true values is not known. While the expression in
N equation 1 (s) is the formal definition of standard deviation, it is easier to
calculate the standard deviation from the following formula:
∑ (x i
− µ )2
N N
σ = i =1
Eq1 ∑ (x − x )2 ∑d 2

N
i i
s= i =1
= i =1 Eq2
N −1 N −1

ii) Variance:
Another way of measuring precision is the variance. The variance is the standard deviation squared (s2).
N N

∑ (x i
− x )2 ∑d 2
i
s2 = i =1
= i =1
Eq3
N −1 N −1

iii) Relative standard deviation, coefficient of variation and confidence interval:

Relative Standard Deviation (RSD): The relative standard deviation can also
Standard deviation in relative terms be expressed in parts per hundred (%) by
is defined as standard deviation multiplying RSD by 100, this is also the Confidence interval
divided by the mean. coefficient of variation, CV. (90, 95 and 99%):

ts
s % RSD = CV
s
*100, pph Confidence interval = x +
RSD = Eq4 x
Eq5
n
x
pph = parts per hundreds or %

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Test for Outlier

Apply a Grubb’s Test and Q-Test for any suspected outliers at 95 % level. See page 83 of text for critical values for 95% confidence.
If your results show an anomalous data then use the Q-test to determine if the result should be rejected.

(Suspected Value - Nearest Value) Eq7 | Questionable value - x| Eq8

Q= G calc =
(Suspected Value - Furthest Value) s

Table of Data, Results and Statistical Analysis: (Data and results for both partner should be reported)
Unknown Raw Data
1. Unknown number= Statistical Analysis
2 Mass unknown (Each trial) 10 Averages and Standard deviations of 7 and 8
3 Mass of crucible (or funnel) and tolerance of final weighing. 11 Variance, RSD and CV for 7 and 8
4 Final Mass of crucible or funnel with precipitate & tolerance. 12 Comparison of Mean with Student’s t (Selected case)
5 Mass of precipitate, each trial 13 90%, 95% and 99 % confidence level
6 Moles of sulfate, each trial
14 Q & G Test (95%) for any outlier.

Analysis and Results

7 Molar mass of sulfate salt (Average)
8 Mass of cation in sulfate salt (Average)
9 Identity of cation in sulfate salt

Discussion
The goal of this experiment was to determine the identity of an unknown metal sulfate salt and to apply statistical analysis on the
results. Write an appropriate discussion for this experiment. Some things to consider in your discussion are: Is the insolubility of the
barium sulfate salt relative to the unknown metal salt critical for this experiment to succeed? Why? Why was excess BaCl2 is added to
the unknown solution. Why is it important to repeatedly weight the crucible and the sintered glass-funnel to constant weight?

Consider the possible scenario. Consider if one of the empty sintered glass-funnel never makes tolerance (0.3 mg) with the other two
funnels making tolerance. In the experiment, there was success in the weighing of the BaSO4 product in two of the three trials (the
sintered glass-funnels that met tolerance). The experiment is not complete, however, until a third result is recorded. How can this
experiment be modified so the third precipitate can be weighed without using a repeating the entire experiment from start?

1 C. H. Hendrickson and P. R. Robinson, J. Chem. Ed. 1979, 56, 341.

2 R. Q. Thompson and M. Ghadiali, J. Chem. Ed. 1993, 70, 170.

Sample Data Table

Sample Unknown # _________ 1 2 3 4
Mass of crucible/funnel (last weighing), (g)
Mass of ppt in crucible/funnel (last weighing), (g)
(A) Mass of ppt, (g)
(B) Moles of sulfate (moles)
Average Standard Variance, RSD
Deviation % RSD (CV)

(C) Formula Weight of unknown sulfate salt

(D) Atomic weight of cation in unknown sulfate salt
Range +/-
Average + -

(E) 90% confidence level

(F) 95% confidence level
(G) 99% confidence level
Questionable
Value QCalc , GCalc New Avg. New Range +/- (95 % CL)

Q-Test Indicate outliner (Atomic weight unknown)

G-Test Indicate outliner (Atomic weight unknown)

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

01 Gravimetric Determination of Molar mass of an unknown sulfate salt ________

% of Score
# CRITERIA (Tentative point distribution - may change depending on experiment) pts % Score
1 Prelab Questions
2 Introduction and Procedures
A. Introduction
• Objective of Expt.
• Background information.
• Math relationship used in study. 10%
B. Procedures
• Outline of procedures in Expt.
• Flow chart pictorial of procedures.
• Procedural changes.
• Information (data) to be recorded during expt. (to be presented in Table form.)
• Safety and disposal information.
This portion of the report should be turned in before the start of lab class (prelab discussion).
3 Data, Observe., Results and Calc.
C. Data and Observation
• Data in table form. & detailed observation written in the table. All data entry should contain the 15%
proper number of significant figures and units. Data should always be recorded in an organize fashion.
• Balance chemical equations; all chemical reaction which occurred during an experiment should be
written in this section. Then it should also be written in the discussion portion of the report.
This portion of the report should be turned in before you leave the laboratory.
Calculations & Results
D. Calculations
• Sample calculation shown 30%
• Statistical analysis of data and result (if applicable)
E. Results
• Result(s) in table form.
In this section accuracy of results is very important as well as detailed calculation showing how the result
was obtain. "Unknown" will also be included in this section.
4 Discussion (Talking points)
F. Discussion
• What is your final result in this experiment. Are the three trials consistent with each other? If not
what would account for the inconsistencies? Were you able to get within 0.5mg in your weighting? If
you had problems, how did you resolve this? 20%
G. Conclusion
• Summary of the goal of the experiment and how that goal was achieved in the experiment.
H Post-lab questions or Editorial comment
• What did you learn in this experiment? What skills in lab practice did you develop through this expt?
This portion (Calculation and Discussion) is turned in at the beginning of class of the due-date
5 Overall Presentation (of lab notebook)
• Lab technique during experiment; example are- class preparation, safety glasses precautions and
leaving the laboratory clean.
• Report presentation: examples are the headings of each report that includes name, title, lab partner, 15%
date and section #.
• Legibility of report. Is the report easy to read or is important information jotted down by small print
in the corners of the lab report? The overall impression is important.
6 Lab Technique 10%
• Safety: wear goggles, handle chemicals with caution, proper handling of lab equipment
• Leave lab clean and tidy

Unknown __________% Error Score ______/___ _______ Student’s t ____/___

Total (This total may be adjusted depending on lab technique and student conduct in the experiment)

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Notes and Modification (Ashless procedure)

The sample is dissolved, if it is not already in solution.

The solution may be treated to adjust the pH (so that the proper precipitate is formed, or to suppress the formation
of other precipitates). If it is known that species are present which interfere (by also forming precipitates under the
same conditions as the analyte), the sample might require treatment with a different reagent to remove these
interferents.

The precipitating reagent is added at a concentration that favors the formation of a "good" precipitate (see below).
This may require low concentration, extensive heating (often described as "digestion"), or careful control of the pH.
Digestion can help reduce the amount of coprecipitation.

After the precipitate has formed and been allowed to "digest", the solution is carefully filtered. The filter is chosen
to trap the precipitate; smaller particles are more difficult to filter.

Depending on the procedure followed, the filter might be a piece of ashless filter paper in a fluted funnel, or a
filter crucible. Filter paper is convenient because it does not typically require cleaning before use; however, filter
paper can be chemically attacked by some solutions (such as concentrated acid or base), and may tear during the
filtration of large volumes of solution.

The alternative is a crucible whose bottom is made of some porous material, such as sintered glass, porcelain or
sometimes metal. These are chemically inert and mechanically stable, even at elevated temperatures. However,
they must be carefully cleaned to minimize contamination or carryover(cross-contamination). Crucibles are often
used with a mat of glass or asbestos fibers to trap small particles.

After the solution has been filtered, it should be tested to make sure that the analyte has been completely
precipitated. This is easily done by adding a few drops of the precipitating reagent; if a precipitate is observed,
the precipitation is incomplete.

After filtration, the precipitate – including the filter paper or crucible – is heated. This achieves three purposes:

The remaining moisture is removed (drying).

Secondly, in some experiments the precipitate is converted to a more chemically stable form. For instance, calcium
ion might be precipitated using oxalate ion, to produce calcium oxalate (CaC2O4); it might then be heated to convert
it into the oxide (CaO). It is vital that the empirical formula of the weighed precipitate be known, and that the
precipitate be pure; if two forms are present, the results will be inaccurate.

The precipitate cannot be weighed with the necessary accuracy in place on the filter paper; nor can the precipitate
be completely removed from the filter paper in order to weigh it. The precipitate can be carefully heated in a
crucible until the filter paper has burned away; this leaves only the precipitate. (As the name suggests, "ashless"
paper is used so that the precipitate is not contaminated with ash.)

After the precipitate is allowed to cool (preferably in a desiccator to keep it from absorbing moisture), it is weighed
(in the crucible). The mass of the crucible is subtracted from the combined mass, giving the mass of the precipitated
analyte. Since the composition of the precipitate is known, it is simple to calculate the mass of analyte in the original
sample.

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

02 Experiment. EDTA Titration of Ba2+ of a) unknown metal sulfate and b) unknown BaCl2
***USE ONLY DEIONIZED WATER (NOT DISTILLED WATER!)THROUGHOUT THE ENTIRE EXPERIMENT***

Objective: The most common multivalent metal ions in natural waters are Ba2+ in the a) filtrate from experiment 1 and b)
an unknown sample. In this experiment, the total concentration of barium ions that can react with EDTA with the
assumptions that EDTA reacts 1:1 with metal (Ba2+) ions.

Equipment Chemicals
250-mL Erlenmeyer flask (3) Buffer (pH 10): Add 142 mL of 28 wt % aqueous NH3 to 17.5 g of NH4Cl and dilute to
50-mL Buret
250 mL with water.
Ring-stand and hardware
Desiccator Eriochrome black T indicator: Dissolve 0.2 g of the solid indicator in 15 mL of
400-mL Beaker triethanolamine plus 5 mL of absolute ethanol. Add a minimum amount of Mg+2 ion so
500-mL Vol. Flask that the indicator starts with a red hue
250-mL Vol. flask
1.0-mL Vol Pipette Test Sample: Filtrate from Experiment 1.
100-mL Grad cylinder
Hot plate Unknowns: 1 L of solution containing 15–25 g of CaCO3 plus 38 mL of 12 M HCl. Each
student will need 100 mL of this solution.

Safety and Waste Disposal

Place all waste in the appropriate waste container. Do not pour any material down the drain. Dispose of nitrile gloves in
the appropriate container.

Discussion: The molar mass of the cation in an unknown sulfate salt was determine by gravimetric isolation in experiment
1. In that experiment, Excess barium sulfate under acidic conditions led to the precipitation of barium sulfate, BaSO4.
The excess barium ions still dissolved in solution remained and was collected as the filtrate.

In this experiment, the Ba 2+ in a) filtrate from experiment 1 and b) an unknown sample, will be determine by titration of an EDTA
titrant. EDTA grabs all the metal ions in the water except group I and NH4+. This causes an experimental error of about 1%, which is
acceptable due to the "fuzzy" endpoints in this type of titration.

EDTA is a versatile chelating agent. A chelating agent is a substance whose molecules

can form several bonds to a single metal ion. Chelating agents are multi-dentate
ligands. A ligand is a substance that binds with a metal ion to form a complex ion.
Multi-dentate ligands are many clawed, holding onto the metal ion to form a very
stable complex. EDTA can form four or six bonds with a metal ion.

Erio-T indicator or Eriochrome Black-T indicator is used in this titration. When it is chelated or acidifies, it produces a Bright Pink-Red
solution. When it is not chelated and under basic conditions it is Blue. The three pictures show the end point in this titration. There is a
1-drop difference of 0.01 M EDTA between the first and second pictures and between the second and third pictures. Two or three
seconds were allowed for colors in the second and third pictures to develop after adding the additional drop. In each case the solution
was thoroughly mixed. This color change from wine red to violet to blue is due to the compact nature of the complex.

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

A weak complexometric indicator name Eriochrome black T (EBT) is added before titration to visualize the presence of barium in
solution. The compound weakly binds to any metal cation (Ba+2) present in solution forming a bright red colored solution. When
eriochrome blact T (EBT) is not bound to the barium ion, it produces a bright blue solution.

Because EDTA is a very strong complexing agent and strongly binds to metals in 1:1 ratio, any metal ions in solution will prefer to bind to
EDTA. The resulting complex, M[EDTA] is colorless. In this experiment, any metal ions bound to EBT indicator will be “stolen” and will
bind to EDTA instead. As EDTA react with the barium in Ba[EBT], the resulting solution changes from red to blue, indicating all barium
has reacted and the reaction is complete.

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

PROCEDURE

A. Titration of an unknown BaCl2 solution.

1A. The EDTA has been prepared and standardize for you. Record the concentration in your notebook.

2A. Before you proceed, you should practice finding the end point several times by adding a little tap water in a clean beaker and
titrating with EDTA. Save a solution at the end point to use as a color comparison for other titrations.

3A. Weigh out the total mass of your solid BaCl2 unknown. Add to a ~100mL volumetric flask and fill to the mark with deionized water.
Mix thoroughly. Be sure that all of the solid dissolves in this stock solution.

4A. Draw 3, 25mL aliquot samples and place each aliquot in 250mL Erlenmeyer flasks. To each sample, add 3 mL of pH 10 buffer and 6
drops of Eriochrome black T indicator. To the first 25-ml solution, titrate with EDTA from a 50-mL buret and note when the color
changes from wine red to blue.

5A. Repeat the titration with the next two remaining samples to find an accurate value of the total % Ba 2+ in the original solid unknown.
Perform a blank titration with 25 mL of distilled water and subtract the value of the blank from each result. Remember that the blanks
are prepared so that they have the same matrix as the actual samples but without the analyte.

B. Titration of filtrate from experiment 1.

6B. Take the filtrate from experiment 1 and make sure that it is in a vessel large enough that it can contain an additional 100mL liquid.
To each sample, add 3 mL of pH 10 buffer and 6 drops of Eriochrome black T indicator. To the first filtrate, titrate with EDTA and
note when the color changes from wine red to blue.

7B. Repeat the titration with the next two remaining samples to find an accurate value of the total % Ba 2+ in the original solid unknown.
Perform a blank titration with 25 mL of distilled water and subtract the value of the blank from each result. Remember that the blanks
are prepared so that they have the same matrix as the actual samples but without the analyte.

8. Upon completion of the experiment, discard all solution in a chemical waste bottle and wash out the glassware. Be sure to dry your
buret in the upside down position.

IMPORTANT NOTE

1. Eriochrome Black T Indicator. The color change of Eriochrome black T at the endpoint is rather subtle. It is not an
abrupt change from deep red to a dark blue; but rather it is from a light red (or pink) to a pale blue. At least one trial
titration is recommended. (You can always discard a "bad" value when you know there is a definite reason for a poor
result. Make sure you indicate a possible problem in your notebook at the time you observe it.)

If you have trouble distinguishing the endpoint, a "before" and an "after" flask are recommended. Prepare two 250-mL
flasks in a similar manner as your samples – except do not add your unknown. Instead, add an equal volume of deionized
water to approximate the volume of the sample aliquot (25 mL), the volume of EDTA titrant that would have been
titrated into the flask. Add the indicator and the ammonia buffer. To one flask (the "before" the endpoint flask) add a
few drops of the Ba solution; to the other flask (the "after" flask) add a small amount of EDTA solution to get just past
the color change at the endpoint. Stopper the flasks and keep them nearby for comparison of the colors. Titrate against
a white background for better discrimination of colors.

Sometimes the Eriochrome black T solution goes bad because of air oxidation. If the endpoints seem very indistinct or
slow to change color to you, try a fresh bottle of indicator. Alternatively, try adding a small amount of solid Eriochrome
black T mixture (1 g indicator ground with 100 g NaCl). A small amount on the end of a spatula is sufficient.

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

_________________________________________________________
Calculations –
Analysis: Analyte Ba2+
The reaction of Ba2+ ions with H2EDTA2- takes place with a 1:1 stoichiometric ratio: Ba2+ + H2EDTA2- D BaH2EDTA.

At the end point of the titration, 1-equivalent of Ba 2+ reacts with one equivalent of H2EDTA2-.

1 eqv Ba2+ = 1 eqv H2EDTA2-; equivalent Ba2+ = [H2EDTA2-] • Vol EDTA

Recall that the analyte (we call this unknown) was prepared by taking all the solid and dissolving it in a 100-mL volumetric flask.
Next a 25-mL aliquot (call this the analyte) of this solution was titrated against EDTA. Note that the analyte moles is equal to
the EDTA moles n at the equivalent point.

A. The mass and % Ba2+ in unknown solid:

Moles of Ba2+ in 25mL Sample = ⎡⎣H 2EDTA2- ⎤⎦ • ⎡⎣Vol EDTA ⎤⎦ = mol H 2EDTA2- = mol Ba2+in 25 - mL Analyte

137.327 g Ba2+
Mass of Ba2+ in 25mL of unknown = mol Ba2+ ⋅ = __ g Ba2+
!##1.0
#"moL
### $
Molar Mass Ba2+

100mL
Mass of Ba in original unknown = g Ba ⋅
2+ 2+
= __ g Total Ba2+
25
# mL
!" #
$
Dilution Fator

Mass Ba2+
Percent Ba in original unknown =
2+
= % Ba2+in unknown
Total Mass Unknown

B. Molar mass of metal sulfate salt from Expt #1 based on back titration of barium.

The excess barium unreacted from experiment 1 is determine from this experiment and subtracted from the total barium that was used
in experiment #1. The difference is the moles of barium that reacted with the sulfate ions in experiment #1 which can be used to
determine the molar mass of the unknown.

Moles of Ba2+ in filtrate = ⎡⎣H 2EDTA2- ⎤⎦ • ⎡⎣Vol EDTA ⎤⎦ = mol H 2EDTA2- = mol Ba2+in filtrate Analyte

___mol BaCl2
Moles of Ba2+used in eperiment#1 = M BaCl2⋅V BaCl2 = ⋅ _ L BaCl2 = ___ moles Ba2+
1-L

Moles of Ba2+ react with SO4 2- in Expt #1 = Moles of Ba2+used in Extp# - moles filtrate from Expt#2

Moles of SO4 2- in Expt #1 = moles Ba2+ reacted with sulfate Expt#2

Mass unk Expt 1

Molar Mass Unknown =
moles Ba2+ reacted with SO4 2- Expt#2

Atomic Mass Unknown Expt #1 = Molar Mass Unknown - Molar Mass SO4 2- ion.

76
Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Statistical Analysis –

1. Report the mean, medium, standard deviations (s), relative standard deviation (RSD), variance (s2) and the 95% confidence

interval for your results.

2. Apply the student’s t test at the 95% confidence interval

3. Apply a Q-test to any suspected result.

4. ts
Confidence interval = x +
n

5. Compare the results of this experiment to the previous experiment, Gravimetric determination of Ca. Apply the

Comparison of Means with Student’s t, Case2 (p76) Comparing Replicate Measurements. Do the two methods agree within

the 95% confidence interval?

Test for Outlier

Apply a Grubb’s Test and Q-Test for any suspected outliers at 95 % level. See page 83 of text for critical values for 95%
confidence. If your results show an anomalous data then use the Q-test to determine if the result should be rejected.

(Suspected Value - Nearest Value) | Questionable value - x |

Q= G calc =
(Suspected Value - Furthest Value) s

Table of Data, Results and Statistical Analysis:

Calcium Raw Data Analysis and Results
Part A Part A
1. Unknown number 12 Mass of Barium in Unknown
4 Concentration of EDTA 13 % of Barium in Unknown (by mass)
5 Mass of Unknown Solid used Part B
6 Volume prepared for Unknown Ba2+ Solution 14 Moles of Barium excess
7 Volume Aliquot for EDTA titration 15 Moles of Sulfate reacted expt #1
5 Volume EDTA during titration 16. Molar mass of Sulfate salt expt #1
6 Volume EDTA for blank trials 17 Atomic weight of cation in metals sulfate
7 Q-Test (95%) of any outlier
Statistical Analysis
PartB
12 Averages and Standard deviations of all results
8. Trial identity for filtrate (1, 2 or 3)
13 Variance, RSD and CV of all results
9. Volume EDTA during titration
14 95% Confidence interval to
10 Volume EDTA for blank trials
15 ttable and tcalc vs expt #1
11 Q-Test (95%) of any outlier

Discussion-
The goal of this experiment was to determine A) amount of barium both in an unknown solid and B) the excess of barium unreacted from
experiment #1 to verify the results from experiment #1. Statistical analysis was applied to the results in this experiment for both
Parts A and B. A discussion of this experiment should include the accuracy and precision of this experiment compared to the EDTA
titration method. An analysis of a comparison of replicated measurement is performed and discussed.

Table of results should include -

Include in your summary table the following:

i) Mass of Ba2+ in the unknown solid and percentage of unknown in the solid.

ii) The molar mass of the unknown sulfate salt and the atomic weight of the cation in the salt.

iv) Mean, standard deviations, RSD and CV for each of the above results.

v) Student’s t at the 95% confidence interval as it applies to the results in this experiment.

vi) Application of a G and Q-test to any suspected result at the 95% level.

vii) ttable, tcalc, Conclusion on comparison of replicated measurements.

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Sample data table.

Sample Unknown # ______ Trial 1 Trial 2 Trial 3 Trial 4 Blank

Mass Na 2EDTA, (g)

Molarity Na2EDTA, (M)

Vol. unknown, (ml)

Buret Volinitial, (ml)

Buret Volfinal, (ml)

Volume EDTA used, (ml)

Vol EDTA for blank, (ml)

Corrected Col EDTA, (ml)

Trial 1 Trial 2 Trial 3 Trial 4 Average Std dev Variance 95% CL

RSD , CV
Mass Ba2+ in 1 ml aliquot (g)

Mass Ba2+ in 1-L solution (g)

Concentration Ca (%)

Concentration Ca (ppm)

Molarity Ba2+, unknown (M)

Mass calcium carbonate in 1L

Q and G Test for Outliner

CaCO3 (g/L), unknown

Student’s t Analysis: Comparing replicate measurements

Analysis A: CaCO3
(g/L) Expt 2 Expt 3 Ex2 (Xi-Xbar)^2 Ex3 (Xi-Xbar)^2
1 Trial 1
2 Trial 2
3 Trial 3
4 Trial 4
Avg

Avg
X1bar - X2bar
Sqrt ((n1*n2)/(n1+n2))
(xi-x1)^2
deg freedom
Spooled

T calc
t table
Conclusion T calc ? T table, at 95%, two result are (not) considered to be different

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

02 EDTA Titration of Ba2+ in an unknown solution.

# CRITERIA (Tentative point distribution - may change depending on experiment) pts Score
%
1 Quiz / Homework [NONE}
2 Introduction and Procedures
A. Introduction
• Objective of Expt.
• Background information. 15%
• Math relationship used in study.
B. Procedures
• Outline of procedures in Expt.
• Flow chart pictorial of procedures.
• Procedural changes.
• Information (data) to be recorded during experiment. (to be presented in Table form.)
• Safety and disposal information.
This portion of the report should be turned in before the start of lab class (prelab discussion).
3 Data, Observe., Results and Calc.
C. Data and Observation
• Data in table form. & detailed observations written in the table. All data entry should contain the proper 15%
number of significant figures and units. Data should always be recorded in an organize fashion.
• Balance chemical equations; all chemical reaction which occurred during an experiment should be written
in this section. Then it should also be written in the discussion portion of the report.
This portion of the report should be turned in before you leave the laboratory.
Calculations & Results
D. Calculations 10%
• Sample calculation shown with Excel spreadsheet available with formulas shown
• Statistical analysis of data and result. Avg, Std dev, RSD, CV
E. Results
• Summary of Result(s) in table form. 20%
In this section accuracy of results is very important as well as detailed calculation showing how the result was
obtain. "Unknown" will also be included in this section.

4 Discussion / Conclusions and Post-Lab Questions

F. Discussion (Talking points)
•What is your final result in this experiment. Are the four trials consistent with each other? If not what
would account for the inconsistencies? How did the results in this experimental result compare to the 20%
result in experiment 2? Is your result for the amount of calcium carbonate in your unknown within the
range of 10 – 25 g/L? Elaborate on this. What is the average amount of calcium in tap water, how much
more higher is this unknown compared to the average content in tap water (express in %).
G. Conclusion
• Summary of the goal of the experiment and how that goal was achieved in the experiment.
H. Post-lab questions or Editorial comment
• What did you learn in this experiment? What skills in lab practice did you develop through this expt?
This portion (Calculation and Discussion) is turned in at the beginning of class of the due-date
5 Overall Presentation (of lab notebook)
• Lab technique during experiment; example are, class preparation, safety glasses precautions and leaving
the laboratory clean. 10%
• Report presentation: examples are the headings of each report that includes name, title, lab partner,
date and section #, witness signature.
• Legibility of report. Is the report easy to read or is important information jotted down by small print in
the corners of the lab report? The overall impression is important.
6 Lab Technique 10%
• Safety: wear goggles, handle chemicals with caution, proper handling of lab equipment
• Leave lab clean and tidy

Unknown __________% Error Score ______/___ _______ Student’s t ____/___

Total (This total may be adjusted depending on lab technique and student conduct in the experiment)

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

03 Experiment. Iodometric Titration of Ascorbic Acid.

The excess starch unknown given to you in this experiment will be used for several experiment so store in a save place.

Objective: The goal of this lab is to determine the concentration of vitamin C in an unknown solid. The analysis will be carried out using
redox reaction of triiodide with ascorbic acid via iodometric titrimetry using starch indicator.

Equipment Chemicals

400mL Beaker
500-mL grad cylinder
(2) 250mL Volumetric flask
50-mL Buret
50-mL Volumetric pipet
25-mL Volumetric pipet
1-L Amber Bottle 3M Sulfuric Acid Potassium iodate, KIO3
500-mL Amber Bottle 1% Starch solution Potassium iodine, KI Ascorbic Acid
(5) 125-mL Erlenmeyer Flask Unknown
50-mL Buret
Pasteur pipet (plastic
Parafilm wax paper

Safety and Waste Disposal: Wear safety goggles and be cautions when working with concentrated acid.

Background Information: Although most mammals can synthesize vitamin-C, or ascorbic acid (C6H8O6), from sugars, man must ingest

considerable quantities of this substance. The National Academy of Sciences recommends the consumption of 60 mg of ascorbic acid per
day. Vitamin-C deficiency, which typically causes abnormalities in bones and teeth, was first characterized in sailors in the eighteenth
century. Compelling sailors to eat limes, a source of vitamin-C, eliminated these abnormalities. Many vegetables also contain large
quantities of vitamin C, but many cooking processes commonly destroy ascorbic acid, and hence citrus fruits are regarded as the most
reliable source of vitamin-C. Vitamin-C can be determined in food by use of an oxidation-reduction reaction. The redox reaction is
preferable to an acid-base titration because a number of other species in juice can act as acids, but few undergoes oxidation of ascorbic
acid by iodine. To prepare the triiodide chemical, a redox reaction between KIO3 (oxidant) and KI (reductant) in acidic medium.

2 KIO 3 (aq) + 10 KI (aq) + 12 H(aq)

+
D 6 I2 + 6 H 2O (l) + 12 K (aq)
+ (1)
(aq)

The solubility of iodine is increased by complexation with iodide to form triiodide:

I2 (aq) + I − ! I3
−
(2)

Triiodide then oxidizes vitamin C to dehydroascorbic acid (not balanced):

C 6H 8O 6 + I−3  C 6H 6O 6 + I− (3)
€
VitaminC dehydroa scorbic acid

As long as vitamin C is present in the solution, the triiodide is converted to the iodide ion very quickly. However, when the all the vitamin
C is oxidized, the triiodide excess will be present, which react with starch to form a blue-black complex.

I3- + starch g iodine-starch complex (blackish-blue color) (4)

Iodine solution is used to test for starch; a dark blue color indicates the presence of starch. The details of this reaction are not fully
known, but it is thought that the iodine (I3- and I5- ions) fit inside the coils of amylose, the charge transfers between the iodine and the
starch, and the energy level differences in the resulting complex correspond to a visible absorption spectrum. The strength of the
resulting blue color depends on the amount of amylose present. Waxy starches with little or no amylose present generally shows red.

Starch indicator is biodegradable and so fresh starch indicator must be prepared after a week of storage. Ask the instructor or lab
tech, when the indicator was prepared before use. Furthermore, although vitamin C is very stable when dry, it is readily oxidized by
oxygen when in solution. Therefore, a solution of vitamin C should not be exposed to air for an extended period of time. Remember that
the molar mass of vitamin-C is 176.12 g/mol.

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

PROCEDURE

Preparation of iodine solution.

1. Dissolve ~ 5.00 g potassium iodide (KI) and ~0.268 g potassium iodate (KIO3) in 200 mL of distilled water in a 400 mL beaker.
2. Add 30 mL of 3 M sulfuric acid. Then pour the solution into a 500-mL graduated cylinder, and dilute to a final volume of 500 mL with
distilled water. Mix thoroughly and transfer to a 1-L brown amber bottle. Degas this solution with nitrogen for at least 5 minutes and
then tightly cap. Wrap parafilm wax paper around the neck of the flask if storing overnight.

Please note: Iodine is very weakly soluble in the water, and can be easily lost from the solution due to its volatility. However, in the
presence of excess iodides, iodine creates I3- ions. This lowers free iodine concentration and such solutions are stable enough to be
used in lab as a titrant. Still, we should remember that their shelf life is relatively short (they should be kept tightly closed in dark
brown bottles, and standardized every few weeks). If you take more than two weeks from when you prepared this solution to the
analysis of your unknown, standardize the iodine solution with ascorbic acid again as discussed in the next procedure.

Preparation of vitamin-C standard solution.

For best accuracy, prepare this solution on the day you are to standardize your iodine solution but no more than a week prior to use. Try
to limit I3- exposure to air as it is oxidized by oxygen. Vitamin-C or ascorbic acid (AA) will oxidize in air (oxygen), so to reduce improve
the accuracy of your iodine standardization, you will to limit the exposure of air to the Vitamin-C solution. Read the literature that
discusses the removal of dissolved oxygen in analytes. (Butler, etal., Talania, Vol 41 No. 2 p211-215, 1994,
https://www.sciencedirect.com/science/article/pii/003991409480110X )

3. Weigh 0.2500 g (to 0.1 mg) vitamin C using an analytical balance and place in a 250-mL volumetric flask. Add sufficient
deoxygenated, deionized water and mix. Finally, dilute to the mark with deoxygenated, deionized water. Store in a clean 500-mL amber
bottle with cap tightly closed wrap with parafilm wax paper if you are to store the solution overnight.
4. In your result page, calculate the formality of this AA solution.

Standardization of the iodine solution with the vitamin C standard solution.

5. Rinse your buret twice with 5 -10 mL of iodine solution, and then fill it. Record your initial buret volume.
6. Collect 25-mL of tap water in a 125mL Erlenmeyer flask then add 10 drops of 1% starch solution to the tap water.
7. Titrate the solution until the endpoint is reached (the first sign of blue color that remains after at least 20 s of swirling). Use this as
a comparison of what the end point should look like for this titration.
8. Take another 125mL Erlenmeyer flask and add 25.00 mL of AA solution (step 3 above). Add 10 drops of 1 % starch solution.
9. Titrate the solution until the endpoint is reached (the first sign of blue color that remains after at least 20 s of swirling).
10. Record the final volume. Repeat this titration at least four times. Results should agree to 0.1 mL.
If you do more than four trials, be sure to label the four trials you will use for your calculations.
11. Finally take 25mL of deionized water add 10 drops of starch and titrate with iodine solution. Correct for the indicator error by
recording the volume of triiodide added in this step and subtract the volume from the end-point volume in step 10.
12. In your result page, calculate (see calculation section):
i) the molarity of iodine solution for each trial.
ii) the average molarity, the standard deviation, RSD, CV and 95% CL for the standard iodine solution.

Preparation of unknown solution.

Again, remember that Vitamin-C is easily oxidized in air. Take the same precaution in preparing your unknown as you did in preparing the
Vitamin-C solution in step 3 above.
13. You will be assigned a solid sample that contains ascorbic acid (record your unknown number in your notebook). Take care to limit the
exposure of your ascorbic acid unknown to air. Also, be sure you same the remainder as this unknown will be analyze in the
electrochemistry experiment and the fluorimetry experiment.
14. Shake your solid sample as thorough as possible. Why is this step important?
Weigh approximately 0.20 g AA unknown solid to the nearest 0.1 mg and report the mass directly in your lab notebook.
15. As in step 3 above, prepare an AA solution in 250-mL volumetric flask. Be sure to use deoxygenated deionize water for this
procedure. Cap the volumetric flask and wrap with parafilm wax paper if you are to store the solution overnight.

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Analysis of Unknown.
16. Using a 50.00 mL volumetric pipet, add 50.00mL of your unknown solution into a 125 mL Erlenmeyer flask.
Add about 10 drops of starch indicator to the sample.
17. Titrate the solution until the endpoint is reached, the first sign of blue color that remains after at least 20 s of swirling
18. Record the final volume. Repeat this titration at least four times. Results should agree to 0.1 mL.
Do not forget to correct for the indicator error after you have completed your four trials.
If you do more than four trials, be sure to label the four trials you will use for your calculations.
19. Use the Grubbs and Q-test (95% confidence level) to check for bad data.
20. In your result page, calculate (see calculation section)
a) the mass of vitamin-C used for each trial
b) the initial volume of the iodine used each trial
c) the final volume of the iodine used for each trial.
d) the total volume of iodine used for each trial
e) the moles of vitamin-C in each trial of the unknown
f) the mass of vitamin-C in the 250mL unknown solution prepared per trial calculated
g) the % m:m vitamin-C in your unknown for each trial of your unknown
h) the average % m:m vitamin-C in the unknown
i) the standard deviation,
j) the RSD or CV
k) the 95% CL for your unknown analysis.
l) Report your final result in the form x + s (n = __), see chapter 4

Turn in the Excel spreadsheet

Calculations-
1. What is the reaction to produce iodine from iodate and iodide? Draw the structures of the organic compounds given in Equation (2).

2. (a) Prepare tables of all your titration data with the following information.
Unknown Information- Iodine Standardization (4 Trials)
Unknown #: Volume aliquot (ml)
Mass Unknown: Vol initial (ml)
Vitamin-C Preparation Vol final (ml)
Mass KI (g) Unknown Titration (4 Trials)
Mass KIO3 (g) Mass Unknown:
Mass Ascorbic Acid (g) Volume aliquot (ml)
Vol initial (ml)
Vol final (ml)

2. (b) Preparation of vitamin C standard solution.

i) Calculate the molarity of vitamin-C standard solution.
2. (c) Standardization of the iodine solution with the vitamin C standard solution.
i) Calculate the molarity of iodine solution for each trial, the average molarity, standard deviation and the rsd.
2. (d) Analysis of Unknown. Calculate the following-
i) the moles of the vitamin-C for each trial for your unknown and the average moles.
ii) the mass of the vitamin-C for each trial for your unknown and the average mass.
iii) the % vitamin-C in your unknown for each trial of your unknown and the average.
iv) the standard deviation, RSD, CV and 95% CL for your unknown analysis.

Statistical Analysis –
i) Report the average, standard deviation (s) and relative deviation (RSD, sr) and the coefficient of variation (CV) and the
95% CL for your result of the vitamin C content in the samples you analyzed.

ii) Apply a Grubbs and Q-test (95% confidence level) for any suspected result.

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Discussion- The main goal of this experiment is to determine the amount of vitamin-C in an unknown solid. Discuss your results (for the

vitamin-C in your unknown) and any source of error that may cause your result to deviate. Discuss the standard deviation of the result

and how the error analysis.

Supplemental Questions (Not required for lab prelab but know how to solve for midterm) -

1. A standard iodine solution was standardized against a 0.4123 g primary standard As4O6 by dissolving the As4O6 in a small amount of

acidic solution and adjusting the pH, see equation (i). If the resulting H3AsO3 solution required 40.28 mL triiodide to reach the end

point, what is the concentration of the triiodide solution?

Reaction: -(i) __ As4O6 (s) + __ H2O g __ H3AsO3 (ii) __ H3AsO3 + __ I3- + __ H2O g __ H3AsO4 + __ I- + __ H+

2. The purity of a hydrazine (N2H4) sample can be determined by titration with triiodide. A 1.4286 g of the oily liquid sample is

dissolved in water and diluted to 100 mL in a volumetric flask. A 50.00 mL aliquot is titrated against the standard triiodide solution in
question 1 (previous problem) requiring 42.41 mL to reach the end point. What is the percent purity by weight of the hydrazine?

Reaction: - (iii) __ N2H4 + __ I3 – g __ N2 + __ I-

3. A 0.200 g sample containing copper is analyzed iodometrically. The titration analysis is prepared by taking copper(II) ion and

reducing it to copper(I) by iodide ions according to the following reaction: (iv) __ Cu2+ + __ I- g __ CuI(s) + __ I2 If the

liberated I2 from this reaction is titrated against 20.0 mL of 0.100 M sodium thiosulfate (Na2S2O3), what is the percent copper in the

sample? The reaction for the titration is- (v) __ I2 + __ S2O32- g __ I- + __ S4O62-

4. Triiodide ions are generated in solution by the following reaction: __ IO3- + __ I- g __ I3-

If a 25.00 mL sample of 0.0100 M KIO3 is added to excess of KI and the product, triiodide, requires 32.04 mL of Na2S 2O3 to reach

the equivalent point, what is the molarity of the Na2S 2O3? Use the equation: __ I3- + __ S2O32- D __ I- + __ S4O62-

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Turn in the following information to you instructor:

Analysis of Vitamin-C by Iodometric Titration

Name: ________________ Mass Unknown _______ Unk # ___________
Vitamin-C Preparation
Mass KI, g
Mass, KIO3, M
Mass Vit-C, g, Standardization reagent
Molarity 250mL Stock Vit-C Standard

Standardization of Iodine
Titration of Vit-C Standards Trial1 Trial2 Trial3 Trial4
Vol Iodine (final) mL
Vol of Iodine, initial (mL)
Vol Iodine, Final (mL)
Vol of Iodine, mL (after correcting for indicator error)

Concentration Iodine solution (M)

Average concentration iodine solution (M)
Standard deviation
Relative Standard Deviation (RSD %)

Titration of Unknown Vitamin-C

Titration of Unknown Trial1 Trial2 Trial3 Trial4
Mass Vitamin-C Unknown (g)
Vol Iodine (initial) mL
Vol Iodine (final) mL
Vol Iodine, mL (after correcting for indicator error)
Mole Vit-C Unknown
Mass Vit C in 250ml Unknown
% Conc. Vit C Unknown
Avg. % Vit-C Unknown
standard deviation
Relative Standard Deviation (RSD %)
95% CL +/- ___ (Avg. +/- CL)

Final Results in form of x + s ( n = __)

% Error Analysis: No not fill g of Vit C g of Total Mix % Vit C % error

#1 Instructor Calculations

Student Calculations

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03 Iodometric Titration of Vitamin-C

# CRITERIA % pts Score

1 Introduction and Procedures
A. Introduction
• Objective of Expt.
• Background information.
• Math relationship used in study. 15%
B. Procedures
• Outline of procedures in Expt.
• Flow chart pictorial of procedures.
• Procedural changes.
• Information (data) to be recorded during expt. (to be presented in Table form.)
• Safety and disposal information.
This portion of the report should be turned in before the start of lab class (pre-lab discussion).
2 Data, Observe., Results and Calc.
C. Data and Observation
• Data in table form. & detailed observation written in the table. All data entry should contain the 15%
proper number of significant figures and units. Data should always be recorded in an organize fashion.
• Balance chemical equations; all chemical reaction which occurred during an experiment should be
written in this section. Then it should also be written in the discussion portion of the report.
This portion of the report should be turned in before you leave the laboratory.
Calculations & Results
D. Calculations
• Sample calculation shown 15%
• Statistical analysis of data and result (if applicable)
E. Results (Complete analysis with Excel spreadsheet)
• Result(s) in table form. Statistical analysis
In this section accuracy of results is very important as well as detailed calculation showing how the result 20%
was obtained. "Unknown" will also be included in this section.
3 Discussion / Conclusions and Post-Lab Questions
F. Discussion
•A complete discussion should be written in this section. Topics to be discuss can be found at the end of
each experimental procedure from the lab manual. Each discussion should include the significance of the 15%
result(s) and the meaning of the result of the experiment. All chemical reactions that occurred during
the experiment should also be included here.
G. Conclusion
• Summary of the goal of the experiment and how that goal was achieved in the experiment.
This portion (Calculation and Discussion) is turned in at the beginning of class of the due-date
4 Overall Presentation (of lab notebook)
• Lab technique during experiment; example are: class preparation, safety glasses precautions and leaving
the laboratory clean.
• Report presentation: examples are the headings of each report that includes name, title, lab partner, 10%
date and section #.
• Legibility of report. Is the report easy to read or is important information jotted down by small print
in the corners of the lab report? The overall impression is important.
Lab Technique
• Safety: wear goggles, handle chemicals with caution, proper handling of lab equipment 10%
• Leave lab clean and tidy
• Time management

Total (This total may be adjusted depending on lab technique and student conduct in the experiment)

Unknown __________% Error Score ______/___ _______ Student’s t ____/___

Total (This total may be adjusted depending on lab technique and student conduct in the experiment)

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

04 Experiment: Quantitative Analysis of Ascorbic Acid Using Cyclic Voltammetry1

You will analyze the ascorbic acid unknown in several experiments so be sure not to contaminate and store properly.

Objective: In this experiment you'll be introduced to cyclic voltammetry techniques to quantify the ascorbic acid content in an unknown
solid. The calibration method used in this experiment is the method of standard additions.

Equipment
1-L reagent bottle (amber)
200mL Volumetric flask
100ml Volumetric flask
(6) 50mL Volumetric flask
Chemicals
10, 15, 20 and 50 -mL vol. pipet 0.10 M phosphate buffer (~450 mL per student)
(6) 20-ml scintillation vials Vitamin-C (Ascorbic Acid)
eDaq Potentiostat Alumina
Pine Printed Screen Electrodes

Safety and Waste Disposal: Wear safety goggles, PPE and be cautions when working with concentrated acid.

Background Information: Electrochemistry comprises a group of important analytical techniques that can provide quantitative
information on the composition of an analyte as well as information about standard reduction potentials and rates of electron transfer
following chemical reactions. Electrochemical detectors are also becoming popular for chromatographic separations. The variety of
information that can be obtained as well as the relatively low cost of the equipment and the convenience of the experiments, make
electrochemical techniques a very versatile and widely used for both qualitative and quantitative chemical analysis.

There are three main types of electrochemical experiments: potentiometry, coulometry, and voltammetry. Potentiometry is the
measurement of the potential of a solution under conditions of low current flow. pH and other ion selective electrodes are common
examples of the use of potentiometry to quantify species in solution. Coulometry involves the quantitative conversion of an analyte via
the transfer of electrons. The total charge or current is monitored as a function of time in a coulometry experiment in order to
quantify the amount of analyte converted. Voltammetry involves the measurement of the current at an electrode as a function of the
applied potential. Although more commonly used for studies of redox potentials and kinetics, special forms of voltammetry can be
effectively used for the quantitative analysis of electroactive species. Polaragraphy and stripping voltammetry, using a mercury drop
electrode, are common methods.

In this experiment, you will use cyclic voltammetry with a printed-screen carbon electrode to determine the percent of the ascorbic
acid in a solid unknown. In cyclic voltammetry, the voltage across the electrode will be varied until the electroactive specie undergoes
electron transfer, which causes a current that is measured across the electrodes. The magnitude of the current is proportional to the
concentration of the electroactive specie.

Ascorbic acid, or vitamin C, is an important nutrient. Various

methods exist for quantifying ascorbic acid in a variety of food.
Although ascorbic acid absorbs light in the UV region,
spectrophotometric methods for the determination of ascorbic
acid in food often suffer from interference due to absorbance
by other components. Acid-Base titration methods are also not
very selective and have rather poor detection limits. Redox
titration using triiodide and starch as an indicator is a reliable
method to quantify the amount of ascorbic acid in a solution.
Chromatography is commonly used with a variety of detectors
including UV and electrochemical. Ascorbic acid is easily oxidized
to dehydroascorbic acid, which undergoes further chemical
reaction to form the gem-diol. The oxidation potential is pH Figure 1. Ascorbic. The first pKa is at 4.17 and the
dependent. In this experiment, the electrochemical reaction can second is at 11.57. (I) The voltammogram under 0.1M
be induced and monitored by voltammetry to quantify the phosphate buffer, pH2.0 and (II) 5mM ascorbic acid in
concentration of ascorbic acid in solution. phosphate buffer, pH 2.0 containing 1mM Na2EDTA.

Review the procedure to use the eDaq Potentiostat and the eChem Software.
http://faculty.sdmiramar.edu/fgarces/LabMatters/Instruments/eDaq/ElectroChem.htm#Operation
Pdf version: http://faculty.sdmiramar.edu/fgarces/LabMatters/Instruments/eDaq/eDaq_Operation/EChemManual.pdf
Set up the eDaq according to the procedure describe in this experiment.

1. W. Okiei, M. Ogunlesi, L. Azeez, V. Obakachi, M. Osunsanmi, G. Nkenchor, Int. J. Electrochem. Sci., 4 (2009) 276-287
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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Procedure
Before beginning this experiment, plan on when you will complete the experiment and sign the log book to reserve the instrument.
All work must be completed by 9:30PM so if you are not prepared at least an hour prior to this time, do not use the instrument.
We start shutting down instruments 15 min prior to the end of the class.

A. Solution Preparations (note: ascorbic acid solutions are oxidized in air, therefore it is recommended that the solutions be remade if
the experiments take more than one day. Use your judgement if you need to do this in this lab.

In order to complete this experiment, you'll need to prepare the following solutions. Before coming to lab, determine how you will
make each of these solutions, including amounts to weigh out and what glassware you'll use etc. An important skill of the analytical
chemist is to know what level of accuracy is required for a given task. Check with your instructor if you're unsure about which
equipment to use. Record your experimental procedure in your notebook and turn in the original pages with your lab report.

1. Measure out 450 mL of the following phosphate buffer solution. Store this in your amber bottle. Be sure the amber bottle is
ultra clean because if you have residual iodine left in your amber bottle it will contaminate the phosphate buffer solution. A 0.10 M
phosphate buffer at pH 2 containing 0.5 g/L Na 2EDTA, available as Na2EDTA·2H2O, will be prepared for you by the lab tech. To
prevent premature oxidation of the ascorbic acid be sure this solution is deaerated prior to use as instructed below. An 80% solution
of phosphoric acid (w/w, r = 1.629 g/ml) and NaH2PO4•H2O are available. When you prepare the solution, first dissolve the
Na2EDTA·2H2O followed by the NaH2PO4•H2O. Only then should you add the acid. Na2EDTA·2H2O will not dissolve otherwise.
Deaerate this solution by bubbling a stream of nitrogen gas through the solution for about 10 minutes.

2. Prepare 200 mL of 10.00 mM ascorbic acid solution using the deaerated buffer solution prepared in step one. To do this,
calculate the mass of ascorbic acid that is necessary for a 10.00 mM, 100mL solution. This solution will be used to practice using the
eDaq potentiostat instrument and also to prepare the standard addition solutions. Keep all solutions tightly closed to minimize air
oxidation of the ascorbic acid. For best results, the solution should be prepared on the same day it is to be used. If this is not
possible, store the solution in an amber bottle (that is free from impurities). Degas the solution and then cap tightly with parafilm
wax wrapped around the seal.

3. Unknown ascorbic acid solution from solid. Mix the solid thoroughly and be sure it is uniform throughout with the inert material.
Weigh around 0.2 g of your unknown to the nearest 0.1mg, place in a 100-mL volumetric flask and then add about 70-mL of 0.10
phosphate buffer made in step 1 above. Deaerate the solution for 10 minutes and then fill to the mark with buffer solution.

Using your three solutions prepare the following in 50mL volumetric flasks:
Solutions Vol. of unknown (ml) Vol. 10.00mM AA solution (mL) Vol of 0.10 M phosphate buffer (mL) **
1 0.00 0.00 50.00
2 10.00 0.00 40.00
3 10.00 20.00 20.00
4 10.00 30.00 10.00
5 10.00 40.00 0.00
(Optimize setting) 6 10.00 40.00 0.00

**Adjust this amount so that the total volume fills the 50mL volumetric flask to the 50mL mark.

B. Setting up the Pine Printed Screen electrodes and connection to the eDaq Potentiostat
The wire harness should be connected to the eDaq potentiostat. If it is disconnected, have your instructor
connect the wire harness to the potentiostat before proceeding. Next take the beige electrode cell cap and
make sure it fits atop the standard 20 mL scintillation vials. A Teflon connector ports sits on top of these
caps. The connector port is blue at the bottom and the printed screen electrodes easily slip at the bottom
of the connector port. These Teflon connectors have a USB Mini-B port, which connects to the wire harness.
See the figure to the right that shows the finally assembly.

A generic cell cable with banana plug termination permits this cell to be used with most potentiostat models.
The banana-plug, color code* is as follows:
WHITE = Reference Electrode RED = Working Electrode
GREEN = Counter Electrode YELLOW = Working Sensor

Once the printed screen electrode is attached, the Teflon connector attached to the electrode cap fits
directly over the 20 mL scintillation vials.

Take 6 scintillation vials and pour about 15mL-17mL each of the solution prepared from above. Add a spatula
of alumina then close the vials with the cap until you are ready to deaerate prior to measuring the cyclic
voltammetry (CV). Prior to measuring the CV of each solution keep the vial under nitrogen. When ready to
measure the voltammogram, place the beige cap over the vial and position the assembly in the glass housing
so that the CV is carried out under nitrogen conditions.

While vial #6 is being scanned, take vial #1 and start deaerating with nitrogen.
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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

C. Initial Electrochemical Set up for Cyclic Voltammetry and

Optimizing the Range parameter.
Your instructor will demonstrate proper handling of the
electrodes and how to use the eDaq potentiostat for
performing the electrochemical experiments. The manual for
the eDaq instrument is in a white binder and is available in the
lab for you to use. The instrument is connected to a printer via
Ethernet from which you can print plots generated by the eDaq
software. The data should be saved in some cloud storge
(Goggle Drive) or a thumb-drive. Do not perform any post data
workup if others are waiting to use the instrument.

First and foremost, sign the logbook. You should sign in the
logbook for each instrument you use. You should also enter in
the logbook the type of analysis to be conducted.

Cyclic voltammetry is often the first electrochemical method chosen to study a system because it can quickly tell you about the
redox potential of the analyte and whether the reaction is reversible or not. When you turn on the eDaq potentiostat for the first
time, make sure the potentiostat’s overload indicator is not lit. If it is a go, to the click on the potentiostat input radio button (see
figure to right) and set the mode to dummy.

The following parameters should be entered under Potentiostat.

The important settings are 20mA range and 10KHz Low Pass. The
invert setting as well as iR Compensation should also be check. Click
OK when done.

Next click on experiment and navigate to cyclic voltammetry.

The following setting should be used under the CV mode.

Start with a scan rate of 50mV/s and use 3 cycles. Make sure the
CV doesn’t have anomalous spikes and that the current doesn’t go off
screen. If this is the case decrease the range under the Input 1:
Potentiostat setting. Change the setting to 50mA and run the CV.
Continue to adjust the range until the current fits in the screen.
Remember that vial #6 will contain the largest concentration of
ascorbic acid so adjusting the range for this solution, will allow all the voltammogram to fit within the screen.

Watch the movie demonstrating how the solutions are deaerate then
position in the degassing chamber as the CV is measured.

D. Cyclic voltammetry for the 5 solutions. Standard addition analysis.

When all the parameters are optimized for vial #6, unscrew the beige
electrode cap from vial #6. Screw the cap on to vial #1 and place in
the degassing chamber. Recap vial #6, then take vial #2 and begin
deaerating the solution while vial #1 is being analyzed. Vial #1
contains just the buffer. This is the blank run and no signal should be
observed. No not change the range setting in the Input1: Potentiostat
menu. For each of the next five vials carry out the following cyclic
voltammetry analysis-

3 cycles at 50mV /s, 3 cycles at 100mV /s and 3 cycles at 50mV/s.

Another option if the voltammogram shows clean signals, is just to do 3 cycles at 50mV and at 100mV. Your instructor can direct
you.

When these scans are complete, remove the vial from the housing, remove the screw cap with the electrodes and exchange the vial
with vial #2. Recap vial #1, start deaerating vial #3 and carry out the CV analysis for vial #2, similar to that of vial #1. As you
measure your CV, none of the setting should be adjusted except for the scan rate, which should be change from 50mV/s to
100mV/s after 3 cycles.

Continue measuring the voltammogram until all 5 vials have been analyzed.
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E. Clean up
Pour all waste in the appropriate mark waste container. Remove the printed screen electrodes from the assembly and place in the
jar labeled spent electrodes. Wash each scintillation vial, dry and return to the vials to your instructor. The vials must be clean
and dry.
If no one else is going to use the instrument after you, log out and sign the logbook indicating the time you used the instrument.

Calculations and Results:

Standard Addition: Calibration curves are used to determine the relation between signal and concentration in quantitative analysis.
Standard addition is used when the sample matrix is complex or unknown. For example, a matrix such as blood has many constituents
that you could not incorporate into standard solutions for a calibration curve. Minimal volume of concentrated standard is added to the
unknown so that the matrix is not changed very much. Matrix effect cannot be corrected for with a calibration curve in which case
standard addition or internal standards is the methods of choice for analysis. In the method of standard addition, a known quantity of
analyte is added to a sample and the increase in signal is measured. The relative increase in signal allows us to infer how much analyte
was in the original specimen. The key assumption is that signal is proportional to the concentration of analyte.

Suppose that a sample with unknown initial concentration [X]i gives a signal Ix where I might be the current intensity, the detector
current or voltage of an instrument. Then a known concentration of standard S (a known concentration of analyte) is added to the
sample and a signal Is+x is observed. Because signal is proportional to analyte concentration, the following equation can be used

Concentration of analyte in Unknown Current from unknown

Concentration of analyte plus standard in mixture = Current from mixture

Standard Addition Equation: [X] i Ix

=
[X] f + [S] f I s+x

Where [X]f is the final concentration of unknown analyte after adding the standard, and [S]f is the final concentration of standard
after addition to the unknown. Note that concentration in these equations can be expressed in either molarity, weight percent or ppm
(ml/L). Be sure to apply the correct conversion when working with either one of these concentration units.

If we began with an initial volume Vo of unknown and added the volume Vs of standard with initial concentration [S]i the volume is V = Vo
+ Vs and the concentration from the above standard addition equation are
#V & #V &
[X]f = [X]i ∗ %% o (( [S]f = [S]i ∗ %% o ((
$V' $V '
Dilution factor Dilution Factor

In this experiment, the amount of ascorbic acid or vitamin-C in your solid sample can be determined by taking electrochemical
techniques. The oxidation
€ of vitamin-C (~0.60 V) is irreversible but the
€ current intensity at this potential can still be used to determine
the concentration of ascorbic acid in the unknown. The analysis will be carried by standard addition. To see an example of the standard
addition calculation, go to page 107 and 108 of the Harris (8th Edition). The standard addition equation for this analysis is derived in the
following manner:

I unk [Vit-C] unk Where, [Vit-C]unk is the concentration of ascorbic acid in the unknown, and [Vit-C]std
= is the concentration of Vitamin-C standard. Iunk is the current of the unknown and
I std + unk [Vit-C] unk + [Vit-C] std
Istd+unk is the current of the vitamin-C unknown and standard solution combination.

In the derivation below, the vitamin-C of your unknown in your solution is represented by [Vit-C]unk. The derivation is for multiple

solutions with constant volume. Rearranging this equation for [Vit-C]unk leads to:

I unk [Vit-C] unk (

I unk [Vit-C] unk + [Vit-C] std ) ! I $
I unk+std = I unk + # unk & ⋅ [Vit-C]
= I unk+std = # [Vit-C] & std
I std + unk [Vit-C] unk + [Vit-C] std [Vit-C] unk " unk %

Plot I unk+std vs [Vit-C] std

(
I unk [Vit-C] unk + [Vit-C] std ) =I I unk+std =
I unk [Vit-C] unk
+
I unk [Vit-C] std

[Vit-C] unk
unk+std [Vit-C] unk [Vit-C] unk ! I $
m= # unk &, b =I
unk
# [Vit-C] &
" unk %

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Note that eqn 1 above is the concentration of the [Vit-C]unk in the scintillation vial (sample
17
that is analyzed). Dilution correction must be applied to calculate the true [Vit-C] y = 2.3143x + 5.7029
15
concentration of the stock solution, which will lead to the % of vitamin-C in the solid unknown. R² = 0.9884
13
Summary:
! I $ 11
I unk+std = I unk + # unk & ⋅ [Vit-C]
std
9
# [Vit-C] &
Main Equation: " unk %
7
Plot: Iunk Vs. [Vit-C]std yields slope of Iunk / [Vit-C]unk 5
Eqn: The x-intercept can be found by setting Iunk+std = 0, which leads to [Vit-C]std = [Vit-C] unk 0.00 2.00 4.00

Report Outline
1. This experiment should be done in triplicate. If this was not carried out then a standard deviation can still be determined with
one sample. The procedure here will allow you to calculate three concentrations of vitamin-C for one standard addition trial.
2. Measured five cyclic voltammogram for five solutions with scan rates of 50mV/s, 100mV/s and 50mV/s, each with 3 cycles.
Complete the table below.
Soln Volume of Volume of 10.00mM Volume of 0.10 M 50mV/s scan rate 100mV/s scan rate 50 mV/s scan rate
unknown Ascorbic Acid phosphate buffer 3 cycles 3 cycles 3 cycles (if complete)
(ml) solution (mL) (mL) Imax1 Imax2 Imax3 Imax1 Imax2 Imax3 Imax1 Imax2 Imax3
1 0.00 0.00 50.00
2 10.00 0.00 40.00
3 10.00 20.00 20.00
4 10.00 30.00 10.00
5 10.00 40.00 0.00

3 Use the second I max2 for each scan rate to carry out your analysis to determine the percent of vitamin-C in your unknown.
4 For the first 50mV/s scan, (yellow highlight), plot I max2 versus [Vit-C]std. From the plot determine the percent of vitamin-C. See
sample calculation below.
5. For the 100mV/s scan, (mustard highlight), plot Imax2 versus [Vit-C]std. From the plot determine the percent of vitamin-C.
6. For the second 50mV/s scan, (orange highlight), plot Imax2 versus [Vit-C]std. From the plot determine the percent of vitamin-C.
7. There should be three plots (see example below) and three vitamin-C concentrations. Calculate an average and apply the
statistical analysis.

Statistical Analysis –
1. Report the mean x, standard deviations (s) and relative standard deviation (RSD)
2. Apply the student’s t test at the 95% confidence interval:
3 Apply a Q-test to any suspected result.
4 Compare the results of this experiment to the previous experiment, Iodometric Titration of Vitamin-C. Apply the Comparison
of Means with Student’s t, Case2 (p76) Comparing Replicate Measurements. Do the two methods agree within the 95%
confidence interval? Are the results between the two experimental protocols statistically different or are the results within
experimental error to each other?

Discussion: Write an appropriate discussion about the is experiment and the advantage and disadvantage of electrochemical techniques
for quantitative analysis.

Compare the procedure in this experiment and the iodometric titration of Vitamin-C. What are the advantages and disadvantages of
each method.

EChem for eDaq Program: You can download program at-

http://faculty.sdmiramar.edu/fgarces/zCourse/All_Year/Ch251/a_LecLab/03_InLab/07_Experiments/04_ElectroChm_VitC/eDaq_%20Software/eDaq%20_Program.zip

You can also go to the course website where you downloaded this
experiment. You will find a link for the eDaq software for both PC
or Mac. Note that the mac version does not support OS Lion 10.6
or higher. If you have MacOS 10.6 or higher you are out of luck
and you will need a mac that uses MOS 10.5 or you can use the CPU
connected to eDaq.

Use the following information when prompt for the License Code.
License Code: NTL2-V7HW-TTCX

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___________________________________________________________________________________________________
Tip sheet

Ascorbic acid standard solution:

• To prepare 1.0 Liter of 0.1 M phosphate buffer take 0.5 g of Na 2EDTA·2H2O, add it to about 600mL of water in a 1-L beaker and stir
until dissolved. Add 13.8 g of NaH2PO4•H2O to the solution and stir until all solid dissolves. Add water so the volume is
approximately 940mL. Add 80% phosphoric acid solution and monitor with a pH meter until the pH reaches 2.0. Stir for an additional
5 minutes to make sure the pH doesn’t drift. Transfer to a 1-L flask and fill to the mark with water.
• The phosphate buffer solution may also be prepared without the EDTA additive since EDTA precipitates at pH lower than 7.65. EDTA
chelates (binds) divalent cations such as Mg2+, Zn2+, and Cu2+. It can be used to make sure there are no free divalent cations in the
solution.
• A 200mL solution of 10.00-mM ascorbic acid solution dissolved in 0.1M phosphate buffer solution at pH 2. This solution is used to
prepare standard solutions ranging from 1, 2 and 4 ppm Vitamin-C. This 10.00 mM ascorbic acid solution is prepared by weighing 352.2
mg of ascorbic acid (176.13 g/mol), placed in a 200mL volumetric flask and diluted to the mark.
• Voltammograms of a solution containing the highest concentration of ascorbic acid is first carried out so that the parameters for the
potentiostat can be optimized. This solution is solution #6 in the table provided in the procedure.
• All solutions should be deaerated with nitrogen (degassed) prior to voltammetry analysis.
• 30-mL and 40-mL volumetric pipets are not available so to deliver these quantities of volume while preparing the standard addition
solutions, use the 15-mL volumetric pipet twice to deliver 30–mL. Similarly, use the 20-mL volumetric pipet twice to deliver 40mL.
You can ignore volume corrections for these pipets.
Below is a sample calculation using Standard Addition at constant volume. This example is for 5.00mM ascorbic acid standard solution.
You will generate a similar plot using 10.0 mM Ascorbic acid solution. You should have three plots so you can calculate three Vitamin-C
percentages.

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APPENDIX

APPENDIX

APPENDIX

APPENDIX

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Lab Practical Chemistry-251 Page 1 of 6

Record your data in your notebook.

Be detailed in your observations.

Use procedure handout as cover page for your report submission.

Save all raw data in the “Chem251_F2018” folder -> LabPractical_F18 and use the filename: lastname_date,

i.e., graces_dec2018

Follow all directions as describe in the procedure handout.

Turn in spectrum and worksheet when you complete the calculations and answer the questions in the

handout.

You should not talk to any other individuals.

You are allowed to ask the instructor or Lab Tech (Afshin) for clarification.

Note: The following pages are subject to change depending on what chemicals will be used for the analysis.
These pages are from last year’s Lab Practical

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Operating the ANASAZI EFT-90 NMR Spectrometer

In this portion of your lab practical you will record the NMR spectrum of an organic compound. You are to operate the instrument
alone. Turn in the spectrum and worksheet at the end of the period. You should not talk to any other individual other than your
instructor or the lab tech for this lab practical. All work should be recorded in your laboratory notebook . Turn in this page as part
of your cover page for your report. It should be the top page. Turn in one report per instrument practical.

Save the raw data in the Chem251_F2018 -> LabPractical_F18 folder with the filename format: lastname_date

Operation Manual. http://faculty.sdmiramar.edu/fgarces/LabMatters/Instruments/NMR/NMR_Operation/NMR_SOP.pdf

I. Procedure Sign in on the log book with the time and date
1. The NMR samples should already be prepared for you in an NMR tube. You will be assigned a sample.
2. Place the sample in the spinner holder and insert in the magnet.
3. Launch the PNMR software and make sure you are observing the 1H nuclei.
4. Shim the magnet to your sample.
5. Set NS (number of scans) to 16
6. Zero-Go (ZG), save your file in the class folder and give it the filename with the format: 1H_lastname_date
(1H_garces_Dec07)
The path is: data -> Chem251_Fall2017. Be sure to save the file in your folder.
7. Upon completion, Open MestReNova, if it is not already open.
Remember that if it doesn’t launch when you click on the icon, go to the Taskbar and quit the program (ask Afshin)
8. Process the spectrum which should include
a) reference peak, b) phasing, c) integration and d) peak pick (See data analysis below for details)
9. Save this processed spectrum in the folder, LabPractical_F17 folder.
10. Print a hard copy, so you can analyze the data and submit with your report.
11. Eject the NMR sample, clean and tidy your work area for the next user. Log out and sign the log book.

II. Data Analysis :

Possible Empirical Formula for your unknown may be: (To be given later)
-When the spectrum is collected, process the data using the following guidelines.
-Fourier transforms the FID to a 1H NMR spectrum.
-Make sure the TMS signal is displayed in the spectrum.
If not, add three drops in the sample and require the spectrum.
-If TMS is not at 0.0ppm, apply the correction so that it is at 0.00ppm.
-Zoom between 10.5 and - 0.5 ppm (You will be plotting this region).
-Label all major signals (Pick Peaks) in the following region:
-Save the workup data using in the Chem251_F17 -> LabPractical_F17 folder with the filename:
lastname_date, i.e., garces_dec2017. Print a spectrum of your results and turn this in with your report.
-Analyze the 1H NMR of your unknown and predict a structure. You should try to rationalize your prediction based on the
information the spectrum shows. Turn in this handout and your lab notebook page with your answer to the questions below.

III. Supplement questions

Analyze the 1H-NMR spectrum to the right.
-The molar mass is ___. The 13C-NMR shows six signals with
one of the signal indicative of a carbonyl. (C=O)
- How many protons are shown in the spectrum to the right?
- What is the chemical shift of the downfield signals?
- What is the chemical shift for the most upfield signal?
- Are you able to see any fine structures (multiplicity) for the
downfield signal? What is the multiplicity?
- From the integrating data, and chemical shift assign the
chemical shift to the protons in the structure and justify
your answer.

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Operating the eDaq Electrochemistry Potentiometer

In this portion of your lab practical you will carry out a cyclic voltammogram of either ferrocene carboxylic acid or potassium
hexacyano iron(III). You are to operate the instrument alone. Turn in your lab notebook pages, the voltammogram and worksheet
at the end of the period. You should not talk to any other individual other than your instructor or the lab tech for this lab practical.
All work should be recorded in your laboratory notebook . Turn in this page as part of your cover page for your report. It should be
the top page. Turn in one report per instrument practical.
Save the raw data in the Chem251_F18 -> LabPractical_F18 folder with the filename format: lastname_date
Operation Manual: http://faculty.sdmiramar.edu/fgarces/LabMatters/Instruments/eDaq/eDaq_Operation/EChemManual.pdf

I. Procedure Sign in on the log book with the time and date
1. Set up the electrochemical cell and use the Pine printed screen electrode and the pattern electrode cell.
2. Use the iron solution that has been assigned to you and fill the glass scintillation vial to the 80% mark.
The cell may already be prepared for you.
3. If already connected, check the wire harness and be sure to have proper connection to the reference, working
and auxiliary electrodes.
4. Degas the sample with nitrogen for 3-5 min.
5. While the solution is being degassed, double-Click the EChem icon on your computers desktop to launch EChem software. When
the software prompts to “scan” turn on the eDaq potentiostat by reaching behind the e-corder 410 to turn on the rocker switch,
the potentiostat will show an overload indicator. Click on “Scan” on the computer at which time the overload signal will turn off.
Never leave the potentiostat with an overload signal. If this happens, click on the right control menu under potentiostat and
change the radio button from Real to Standby . If this doesn't turn off the overload signal, set the status to "Dummy".
7. Adjust the band pass filter and current range so that the voltammogram is not noisy but takes up the full screen when you run
the scan. Adjust the range so the voltammogram fills the screen. You will need to adjust this later after recording a
voltammogram.
8. From the techniques menu select Cyclic Voltammetry and set up the scan so that the scan range is centered around E1/2. See
the voltammogram below for what the voltammogram format. Initially apply the following settings: Ramp: Initial -1000mV,
Ramp Rate 100mV/s, Ramp Width 20ms, Limits: Upper and lower limit (You decide), No. cycles 3, Sampling period 5ms, Rest
Time 5s. Adjust other settings as necessary until all impurities are eliminated and so that the cathodic and anodic scans are
centered around E1/2. You can do this by narrowing your scan window and changing the initial Ramp by adjusting the Upper and
Lower Limits of the scan.
9. When you are satisfied with your voltammogram of iron complex, save the raw data in the “Chem251_F14” folder and use the
filename: lastname_date, i.e., graces_dec2017. Your results should look like the voltammogram shown below.
10. Process the spectrum as directed below and also turn in a copy of your result.
(The instrument is now able to print to the LaserJet printer in the instrument room.)
11. When done, log off the computer, turn off the potentiostat and clean the cell and the patent electrodes.
Dispose of the electrode in the waste container provided at the station.
12. Turn in a hard copy of the voltammogram, this handout and your lab notebook page with your answer to the questions below.

II. Data Analysis (You may elect to determine the values here if you have time on the instrument)
•Label the hard copy of the voltammogram and write any pertinent information on the spectrum.
•Which iron compound did you analyze?
•Label the voltammogram with the following information: Epc , Epa, E 1/2, ipc, ipa, Epp

•Print a hard copy of your spectrum and turn it in with your report.

III. Supplement Question .

Is the voltammogram of your sample reversible? How many electrons are involved in the redox process?
If a voltammogram of a more concentrated sample of Iron (III) sample were measured and you kept the same settings as describe
in this experiment, which of the six measurements (Epc, Epa, E 1/2, ipc, ipa, Epp) would change? Discuss if it would go up or
down from its original value and explain.

[ Ferrocene carboxylic acid ] [ K3Fe(CN)6 ]

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Operating the HORIBA Jobin Yvon Fluorolog-3 Spectrometer

This portion of your lab practical you will record the Fluorescence spectrum of quinine. You are to operate the instrument alone.
Turn in spectrum and worksheet at the end of the period or when done writing up your report. You should not talk to any other
individual other than your instructor or the lab tech for this lab practical. All work should be recorded in your laboratory notebook .
Turn in this page as part of your cover page for your report. It should be the top page. Turn in one report per instrument
practical. Save the raw data in the Chem251_F18 -> LabPractical_F18 folder with the filename format: lastname_date
Operation Manual: http://faculty.sdmiramar.edu/fgarces/LabMatters/Instruments/FluoroSpex/Fluorimeter_Operations/Flurolog_Operations.pdf

I. Procedure Sign in on the log book with the time and date

1. Instrument should already be turned “on” for you.

2. Check to make sure that the cuvette holder is clean there are no cells in the holder.
3. Launch the software for the Fluorimeter (FluorEssence).
4. Make sure the instrument initializes before moving on to the next step. If the instrument does not initialize, log off the
software and launch the software again.
(The next series of instruction is optional and need not be run if the instrument has already been warmed up for you)
5. Run the excitation calibration check.
Save the data in the folder Chem251_F18 using the filename: lastname_dateLampX, i.e., graces_Dec18_LampX
Be sure that the strongest signal in the excitation scan is centered around 467nm.
6. Run the emission calibration check using HPLC quality water to check the water-Raman line
This sample should be found in a cuvette cell near the instrument. Record the CPS (counts per sec) intensity for this signal
in the datasheet and record in the log book. Save the data in the folder Chem251_F18 -> LabPractical_F18 with the
filename: lastname_dateH2OM
7. You have quinine standard solution available as well as a quine unknown. You can use all the standards or just part of the
standards, you can decide as to what will give you the best result for the time you invest. You will ultimately determine the
concentration of the unknown quinine solution assigned to you.
a) Run the emission scan with ex = 350nm. Instead of just monitoring em = 450nm, set up the emission to monitor
between 400nm – 550nm and change the emission slit to an appropriate value based on your experience in this course. For
each analysis, save the files in the appropriate folder with the filenames: lastname_date_0.1ppm, lastname_date_0.5ppm
…, lastname_dateUnk
b) When you have completed the experiment, process the data as described below.
If you have time generate a stack plot and print the graph.
8. Log off the computer and sign out in the log book but do not turn off the computer.
9. Clean up your work area.
10. Turn in this handout and your lab notebook page with your answer to these questions.

II. Data Analysis

• Use the cursor function to find = 450nm.
• Record the CPS (intensity) at the wavelength for your standards.
• Using the data above, carry out the analysis using Excel.
• Use LINEST for all the statistical information.
• Determine the concentration of your unknown with standard deviation.
• Print a hard copy of your spreadsheet and the fluorescence spectrum.
Be sure to write proper headings and labels in your graph.

III. Question
Why is it plausible to just monition the emission at = 450nm in this
experiment instead of the 400 – 500nm range? What are possible errors
that could occur if the concentrations were greater that 1 ppm? Why is it
necessary to calibrate the excitation and emission of the fluorimeter at
the start of this expeirment?

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Operating the ThermoScientific GCMS (GC-FID mode)

In this portion of your lab practical you will determine the concentration of cyclohexane in a cyclohexane-toluene mixture. The
instrument will plot the area under the curve of the cyclohexane chromatogram for your standards and unknown. Use this data to
plot a calibration curve and to determine the concentration of your unknown. You are to operate the instrument alone. Turn in a
copy of the report with other required material at the end of the period. You should not talk to any other individual other than
your instructor or the lab tech for this lab practical. All work should be recorded in your laboratory notebook . Turn in this page as
part of your cover page for your report. It should be the top page. Turn in one report per instrument practical.
Save the raw data in the Chem251_F18-> LabPractical_F18 folder with the filename format: lastname_date

Operation Manual: http://faculty.sdmiramar.edu/fgarces/LabMatters/Instruments/GC/GC.htm#Operation

I. Procedure Sign in on the log book with the time and date
In this experiment, the optimum parameters have been set up for you. You will just need to initiate the sequence assigned to you.
The name of the sequence will be LP_yourlastname.
Sign in on the log book with the time and date
1. Check to make sure the auto sampler is in good condition, then place the standards and the unknown assigned to you in the
carousel. Note the position because you will need to input the position in the method developed for this experiment under
“data”.
2. Click on the desktop icon, Chromeleon, then click on instruments and then the FID tab to make sure the FID is on. If not,
click on the radio button for temperature, wait until the temperature reaches 280°C, then click on the radio button for the
flame, hydrogen air and Makeup gas. Listen for the “pop” near the syringe inlet, this means the FID has been ignited. Now
you can click on Data. The lab tech will be present to assist if there are difficulties with this procedure.
5. Under Data, look at the left menu for the path, Afshin -> GC-FID -> Fall 2018 -> LabPractical_F2018, find the injection
sequence file created for you. Click on that file and upon opening, update the position for the vials and change the status
from Finish to Idle.
6. If everything is update, click on the first sequence once and then click on Start at the top of that window.
7. When the analysis is complete, double click on the first injection sequence and make sure the chromatogram has been
integrated. If it all checks, you can proceed with generating the report.
8. With this window still open, click on Data Processing, then Electronic report.
Choose, Overview, Integration and Summary. Leave the other radio box blank. Click on Finish and then print the report.
9. Log off the GC program and clean up your work area. Leave the GC instrument on for the next student.

II. Data Analysis

• Using the data above, carry out the analysis using Excel.
• Use LINEST for all the statistical information.
• Determine the concentration of your unknown and include the standard deviation.
• Print a hard copy of your spreadsheet and copies of the Chromeleon report.
• Turn in this handout and your lab notebook page with your answer to these questions.

III. Question
What is the retention time for the cyclohexane and toluene peak? Calculate the values.
If these peaks were not resolved, what is the procedure to improve the resolution of the chromatogram peaks?
What other method that we did this semester can be used to determine the concentration of toluene and cyclohexane in a
mix?
Explain your rational

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The protocol will be given sometime in November

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Appendix 1
Care and Handling of Chemicals

The success of a chemical reaction or analysis is critically dependent on the purity and quality of the chemicals used. Thus, it is of utmost
importance that the chemicals supplied for an experiment be of sufficient purity for the experiment to work and that contamination of
these chemicals do not occur during the course of a laboratory.

Grades of Chemicals: Chemicals are available from suppliers in a number of different grades of purity. The least pure (and also the
cheapest grade) is technical grade. This grade of chemical should only he used when contamination is not important or in the initial stages
of washing glassware. The most commonly used grade is A.C.S. reagent grade. These chemicals must meet minimum purity standards, which
are specified by the American Chemical Society. Reagent grade chemicals are appropriate for all but the most exacting or specialized
work. The highest grade of purity is primary-standard grade. These chemicals must he extraordinary pure and extremely stable, and are
used when the highest possible accuracy is needed. Some chemicals may also be used for special purposes and are called specialty grade
chemicals. Solvents may he specially purified to eliminate light absorbing impurities (spectrophotometric grade) or to eliminate particulate
matter (HPLC grade). Specific impurities may be eliminated to enhance the usefulness of the chemical for some specific reaction with
which the impurity would interfere. As the cost of a chemical is much greater the higher its purity, only the grade actually needed for
the experiment to work is used. Thus, primary-standard grade chemicals are not used for all reactions.

Avoiding Contamination of Chemicals: It is absolutely essential that chemical reagents not become contaminated during the course of
the entire laboratory sections conducted for each experiment. In order to avoid this, it is very important that the following simple rules
he observed:

1) Only take as much of a chemical as you need for the experiment.

2) Never put any excess chemical back into its container. Dispose of it instead.
3) Never place the bottle lid or stopper on the bench top where it may become contaminated. Hold it in your hand or place it on a
clean Kim-wipe. Replace the top immediately after use.
4) Never stick a metallic object into a chemical bottle. If the solid inside is not free-flowing gently tap it against the countertop to
loosen the solid. If this does not work, a clean porcelain spoon or glass stirring rod may be used to break up the solid. Be careful not
to break the rod!

______________________________________________________________________________________________

Appendix 2
Measurement of Mass

Introduction: While a variety of different types of balances exist for the measurement of the mass of a sample, by far the most common
today and the one used in this course is the single pan top-loading electronic balance. These balances are quite accurate, with a quality
balance measuring to the nearest 0.0001 g. They are also both fast and easy to use. However, as with any piece of electronic equipment
they are quite delicate and should be treated with care.

General Considerations: There are a number of general considerations that apply to the use of balances to measure mass. Glassware
whose mass is to be determined should be clean, dry and at room temperature. Chemicals to be weighed are never placed directly on the
balance pan: instead they should be weighed into the container in which they will be used or weighed using weighing paper. If the chemicals
are hygroscopic (they absorb water from the atmosphere), they must first be dried in an oven and then cooled in a desiccator before
weighing. If the balance has an enclosed chamber all doors must be closed for any weighing operation. The object(s) being weighed must
not touch any surface besides the balance pan.

Mettler Balance: If the balance is not already switched on, make sure all of the doors (if any) are closed and then turn it on by depressing
the lever in the front. After a short period of time a reading of zero mass should appear in the scale. If any other number appears depress
the lever again. If the numbers on the scale are rapidly changing or if anything else appears on the scale, consult the instructor. If an
object is to be weighed, place it on the pan (opening and closing the doors if necessary) and take the reading. If a chemical is to be
weighed, place the container or weighing paper of the pan and depress the lever again. This tares (re-zeros) the balance so that the weight
of the container or paper is not included in the reading. Slowly add the chemical to the container or paper until the desired weight is
reached. Record the exact value used. If the experiment calls for 2.0 + 0.1 g, don't waste your time trying to get exactly 2.0000 g. Any
value between 1.900 and 2.100 g is acceptable as long as you know exactly how much you used. Any chemical spilled must be immediately
swept out of the chamber using the brush found on top of the balance.

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Appendix 3
The Measurement of Volume

General Considerations
The quantity of liquid used in an experiment is conveniently measured by the volume it occupies. How this volume is measured depends
upon how accurately the volume needs to be known and whether a fixed or variable quantity of liquid is needed. The most commonly used
units for volume are the liter (L), which equals 1 cubic decimeter by definition, and the related milliliter (mL), which is one-thousandth
(1/1000) of a liter. 1 mL = 1cm3 = 1 cc (cubic centimeter)

There are three general considerations to keep in mind when measuring the volume of a quantity of liquid. First, the glassware used must
be clean. Liquid droplets usually adhere to dirt or films on the glassware, so the amount of liquid delivered when the liquid is transferred
from the measuring container is too small. Second, in a piece of glassware with a narrow bore such as a buret or a pipet the surface of
the liquid will not be perfectly flat. If the intermolecular forces between the liquid molecules are less than those between the liquid
molecules and the glass, a concave meniscus will develop. This is the case for water and glass. By convention we measure the volume of the
liquid at the bottom of a concave meniscus us. If the intermolecular forces between the liquid molecules are greater than those between
the liquid molecules and the glass, a convex meniscus will develop. The volume at the top of the convex meniscus is read.

Third, the eye of the observer must be at the same level as the meniscus in order to avoid parallax error. Parallax is the apparent
displacement of a liquid level as an observer changes position. It occurs when the observer's line of vision is not perpendicular to the
surface of the calibrated scale being read and is a result of the refraction of light by the glass and the liquid.

Glassware
A. Beakers and graduated cylinders: When the volume of liquid used needs to be only approximately beakers or graduated cylinders
may be used. Liquid is poured into the glassware until the volume desired is reached as determined by using the scale imprinted on
the side of the glassware. The volumes obtained may be off by as much as 20% in the case of beakers, so only noncritical volumes
should be measured in this way.

B. Volumetric pipets: Volumetric pipets are used to deliver a fixed, accurately known volume of liquid into a container. They are
available in a variety of sizes between 0.5 and 200 m L, with larger pipets having the best relative accuracy.

Volumetric pipets are used with rubber bulbs according to the following procedure:
A small volume of liquid is drawn up into the pipet using a rubber bulb. The bulb is removed and the liquid is then used to thoroughly wet
the interior surface of the pipet. This liquid is drained out. The bulb is reattached and liquid drawn into the pipet until it is above the
pipet mark. Raise the pipet above the level of the liquid and wipe off any drops adhering to the outside. Replace the bulb with a moistened
forefinger. Slowly let the liquid drain back into its original container until the bottom of the meniscus is at the mark. Move the pipet to
the receiving container and let it drain. When liquid flow ceases touch the pipet tip to the inside wall of the container. Let the tip rest
there for at least 10 seconds. Remove the pipet from the container. Do not blow out the small remaining volume in its tip.

Volumetric pipets are used with suction bulbs by the same basic procedures, with the following changes:
In order to create suction the 'S" bead is squeezed simultaneously with the bulb. Release the bead first. Attach the bulb to the pipet.
Squeeze the "S" bead to suction liquid into the pipet. Squeeze the "E" bead to lower the liquid level in the pipet without removing the bulb.

Volumetric pipets are used with pipet pumps as follows:

Hold the pipet close to its upper end and insert it into the opening of the pump using slight pressure and a twisting motion. Submerge the
end of the pipet into the solution and turn the wheel with your thumb. Draw fluid up to the mark. To expel turn the wheel in the other
direction or push the plunger down.

Under no circumstances are you to pipet by mouth!

C. Burets are used when an accurately measured volume of either a quantity of liquid which is not known at the beginning of the
experiment or a known volume which does not correspond to any available volumetric pipet volume needs to be delivered to a container.
Buret volumes are measured by difference. A reading is made of the initial volume, followed by a reading of the final volume, and the
volume delivered found by subtraction. It is important to know that buret volumes are read to the nearest 0.01 Iii on typical 50 'mL
burets, and that the buret scale has 0.0 iii at the top and 50.0 mL at the bottom.

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Burets are used as follows:

Between 5 and 10 mL. of the liquid that will fill the buret are placed in it. This liquid is swirled around inside the buret to rinse and coat
all surfaces, and then drained out the tip. Repeat this step. Fill the buret above the zero-mark using a funnel to avoid spillage. Drain liquid
through the tip to fill it and displace any air bubbles in the stopcock until the liquid level is at or just below the zero mark. Record this
initial volume. Move the receiving container under the buret tip. For dispensing a known volume of liquid open the stopcock until the desired
liquid volume is obtained. Record the final buret volume and be sure to use the volume actually delivered in your calculations. For titrations
add liquid to the container slowly to ensure that the endpoint is not overshot. Any liquid which splashes onto the sides of the container
may be rinsed down with solvent Partial drops from the buret may be added to the flask by letting a small amount of liquid hang from the
tip of the buret, touching the container wall to the tip, and then rinsing the wall with solvent. Record the buret reading at the endpoint
and find the volume used by difference.

D. Volumetric Flasks: In preparing solutions of known molarity the final volume of the solution must be known since molarity is
defined as moles of solute per liter of solution. Volumetric flasks are used for this purpose. They are only used to contain a known
volume and never to deliver liquid.

Volumetric flasks may be used according to the following procedure:

Fill the volumetric flask between one-half and two-thirds full with liquid. Quantitatively transfer the desired quantity of solid into it using
a powder funnel. Rinse the powder funnel with liquid to insure all of the solids went into the flask. Swirl the flask to aid in the dissolving
of the solid. After it is all dissolved fill the flask to the mark, using an eyedropper to add the last few drops. Be careful not to overshoot!
Stopper the flask and invert it several times to thoroughly mix the solution.

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Appendix 4
Titration Technique

Burets are long, narrow, finely graduated tubes as shown in the figure.1. They are designed to deliver precise and variable volumes of
liquids into other containers. A stopcock or pinch clamp at the base of the buret provides for release of volumes between about 0.05
mL and the total volume of the buret. Burets are especially useful for adding solutions stepwise in small increments. Burets typically
have uncertainties of about + 0.1%. Thus, you might measure 21.33 + 0.02 mL using a buret.

The steps for using a buret are illustrated in the figure .2 provided. First secure the buret in a buret clam attached to a ring stand (1) .
If you have never used a buret or have only used it a few times, it is wise to practice manipulation of the stopcock or pinch clamp to
adjust the liquid flow using deionized water. Partially fill a clean buret with deionized water. Then adjust the stopcock or pinch clamp a
number of times until you have the feel of the degrees of turn or pressure required to release liquid one drop at a time or in a steady
flow. The stopcock should be handled with the thumb and two fingers (2) along with a slight inward pressure on the plug to prevent
leakage. The pinch clamp should be handled with the thumb and third finger. Do not use the buret for the actual experiment until you
are conformable carrying out these operations with relaxed muscles.

Fill a clean buret that has already been rinsed with your reagent solution with a few more milliliters of solution than you need for the
task at hand (3). Then open the stopcock or pinch clamp long enough to fill the buret tip (2). Since the volume of solution delivering by
the buret is always determined by taking the difference between an initial volume and the final volume, it is not necessary or even worth
the effort to adjust the initial reading to the zero-calibration mark. Therefore, record the initial volume whenever it is by observing
the position on the graduated scale of the lowest portion of the meniscus (4). Make certain that your eye is at the same level as the
meniscus (5). A dark background placed behind the buret and at or just below the meniscus makes it easier to read (6).

Place the receiving flask under the buret and over the white paper that enhances visibility at the end point. Make certain that you have
added the required drops of an indicator solution if you are performing an acid-base titration or an oxidation-reduction titration. Open
the stopcock or pinch clamp carefully to adjust the liquid flow from dropwise to a rapid flow as desired (7). When as much solution as is
needed has been delivered, close the stopcock or pinch clamp, and touch the inner wall of the receiving container to the buret tip to
remove any hanging drop (8). If you are using the buret for titration to an endpoint, then rinse the wall of the receiving flask with
deionized water (9), and record the final volume by observing the new position of the meniscus. If you are using the buret not for
titration to an endpoint, but simply to deliver a carefully measured volume of a liquid, do not rinse the wall of the receiving vessel with
deionized water before observing and recording the final volume.

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Appendix 5
Using CARY UV-VIS Program to Analyze

Cobalt Chloride Hexahydrate Solutions

1. Go into program “Cary UV VIS.”

2. Select SCAN submenu.

a. Select “Set up” submenu.
b. Set minimum and maximum wavelengths. (700nm left window, 400nm-right window)

3. Baseline menu(sets zero and 100%T)

a. Select “zero/baseline” option, click okay.
b. Select Zero menu button and then :select Baseline.” Insert Blank. Click Okay.
c. Prompts for blocking the beam (block beam with a solid dark colored plastic item).

4. Ready to scan samples.

a. Hit Start
b. Insert maximum strength standard (highest conc, darkest color.) with small arrow on left of cuvette facing leftward:<
c. Instrument will ask for “Filename.” Enter one.
d. Instrument will ask for sample. (optional—hit cancel).
e. Click okay.
f. Instrument will perform scan and display a graph of this output.
g. Select xy button, second from right, above graph. Select x label and hit okay. The graph will be labeled with the l max.
(This is the wavelength setting you will set below to scan standards and samples.)
h. Close Cary UV-VIS window.(exits scan subprogram)

5. Ready to analyze a set of samples:

a. Re-open Cary UV VIS program.
b. Select Conc submenu. (or “Sunglasses” for that experiment) Instrument will calibrate (noise).
c. Select “Set up” submenu.
d. Set analysis wavelength to the max found in 4g. (e.g. ~510nm for CoCl2•6H20.)

6. Select “Standards” from Analysis submenu.

a. Set units (e.g. g Co/25mL H2 O), enter concentrations of Cobalt standards. Select “linear” fit type, click okay.
b. Click Zero button: Load Blank and click “okay.” Instrument will scan blank.
c. Click Start.
d. Select solutions to be analyzed from “Standard/Sample Selection” menu Click okay.
e. Type in a filename. Click okay. Instrument will now prompt you to insert standards and then the samples. (Insert standards and sample
cuvettes from lowest to highest concentration after prompted, and after inserting each of the cuvettes click okay (e.g., standards a, b,
c, d, e and samples 1, 2, 3).

7. R2 Min FAIL: If this yellow attention box is displayed after you have run all your standards, they are not in increasing concentration
sequence. Click okay. Look at the graph. See which point is out of order on the graph, then reorder standards in correct sequence.
b. Click Re-Read button left of graph, and the instrument will prompt you to re-insert your samples as in step 6e.

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Appendix 6
Electromagnetic Spectrum

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Appendix 7
Physical Properties of H2O
DENSIY OF WATER FROM 0 °C TO 40 °C
°C g / mL °C g / mL °C g / mL
0 0.999 868 5 0.999 992 10 0.999 728
1 0.999926 6 0.999968 11 0.999634
2 0.999968 7 0.999930 12 0.999526
3 0.999 992 8 0.99 876 13 0.999 406
4 1.000000 9 0.999809 14 0.999273
°C 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
15 0.999 129 0.999 113 0.999098 0.999083 0.999067 0.999052 0.999036 0.999020 0.999004 0.998988
16 0.998 972 0.998 956 0.998 939 0.998 923 0.998 906 0.998 890 0.998 873 0.998 856 0.998 839 0.998 821
17 0.998 804 0.998 787 0.998 769 0.998 752 0.998 734 0.998 716 0.998 698 0.998 680 0.998 662 0.998 643
18 0.998 625 0.998 606 0.998 588 0.998 569 0.998 550 0.998 531 0.998 512 0.998 493 0.998 474 0.998 454
19 0.998 435 0.998 415 0.998 395 0.998 375 0.998 356 0.998 336 0.998 315 0.998 295 0.998 275 0.998 254
20 0.998 234 0.998 213 0.998 192 0.998 171 0.998 150 0.998 129 0.998 108 0.998 087 0.998 065 0.998 044
21 0.998 022 0.998 000 0.997 979 0.997 957 0.997 935 0.997 912 0.997 890 0.997 868 0.997 846 0.997 823
22 0.997 800 0.997 778 0.997 755 0.997 732 0.997 709 0.997 686 0.997 662 0.997 639 0.997 616 0.997 592
23 0.997 568 0.997 545 0.997 521 0.997 497 0.997 473 0.997 449 0.997 424 0.997 400 0.997 376 0.997 351
24 0.997 327 0.997 302 0.997 277 0.997 252 0.997 227 0.997 202 0.997 177 0.997 152 0.997 126 0.997 101
25 0.997075 0.997049 0.997024 0.996998 0.996972 0.996946 0.996920 0.996893 0.996867 0.996841
°C g/mL °C g / mL °C g / mL
26 0.996 814 31 0.995 372 36 0.993 716
27 0.996544 32 0.995058 37 0.993360
28 0.996264 33 0.994734 38 0.992997
29 0.995976 34 0.994403 39 0.992626
30 0.995678 35 0.994064 40 0.992247
These densities, given in g / mL, can be converted to g / cm3 by multiplying each value by 0.999 972.

VAPOR PRESSURE OF WATER

T P T P T P T P
°C torr °C torr °C torr °C torr
19.1 16.581 22.1 19.948 25.1 23.897 28.1 28.514
19.2 16.685 22.2 20.070 25.2 24.039 28.2 28.680
19.3 16.789 22.3 20.193 25.3 24.182 28.3 28.847
19.4 16.894 22.4 20.316 25.4 24.326 28.4 29.015
19.5 16.999 22.5 20.440 25.5 24.471 28.5 29.184
19.6 17.105 22.6 20.565 25.6 24.617 28.6 29.354
19.7 17.212 22.7 20.690 25.7 24.764 28.7 29.525
19.8 17.319 22.8 20.815 25.8 24.912 28.8 29.697
19.9 17.427 22.9 20.941 25.9 25.060 28.9 29.870
20.0 17.535 23.0 21.068 26.0 25.209 29.0 30.043
20.1 17.644 23.1 21.196 26.1 25.359 29.1 30.217
20.2 17.753 23.2 21.324 26.2 25.509 29.2 30.392
20.3 17.863 23.3 21.453 26.3 25.660 29.3 30.568
20.4 17.974 23.4 21.583 26.4 25.812 29.4 30.745
20.5 18.085 23.5 21.714., 26.5 25.964 29.5 30.923
20.6 18.197 23.6 21.845 26.6 26.117 29.6 31.102
20.7 18.309 23.7 21.977 26.7 26.271 29.7 31.281
20.8 18.422 23.8 22.110 26.8 26.426 29.8 31.461
20.9 18.536 23.9 22.243 26.9 26.582 29.9 31.642
21.0 18.650 24.0 22.377 27.0 26.739 30.0 31.824
21.1 18.765 24.1 22.512 27.1 27.897 30.1 32.007
21.2 18.880 24.2 22.648 27.2 27.055 30.2 32.191
21.3 18.996 24.3 22.785 27.3 27.214 30.3 32.376
21.4 19.113 24.4 22.922 27.4 27.374 30.4 32.561
21.5 19.231 24.5 23.060 27.5 27.535 30.5 32.747
21.6 19.349 24.6 23.198 27.6 27.696 30.6 32.934
21.7 19.468 24.7 23.337 27.7 27.858 30.7 33.122
21.8 19.587 24.8 23.476 27.8 28.021 30.8 33.312
21.9 19.707 24.9 23.616 27.9 28.185 30.9 33.503
22.0 19.827 25.0 23.756 28.0 28.349 31.0 33.695

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Appendix 8
Acid-Base Indicator

http://chemistry.about.com/library/weekly/aa112201a.htm

pH Hydro-ion paper indicator

Cabbage Indicator

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Appendix 9
Acid Dissociation Constant, Ka @ RT. (These values may vary depending on the source used)
Acid Formula Ka1 Ka2 Ka3
Acetic CH3COOH 1.75x10-5

Ammonium Ion NH4+ 5.70x10-10

Anilinium Ion C6H5NH3+ 2.51x10-5
Arsenic H3AsO4 5.8x10-3 1.1x10-7 3.2x10-12
Arsenous H3AsO3 5.1x10-10
Benzoic C6H5COOH 6.28x10-5
Boric H3BO3 5.81x10-10
1-Butanoic (butric acid) CH3CH2CH2COOH 1.52x10-5
Carbonic H2CO3 4.45x10-7 4.69x10-11
Chloroacetic ClCH2COOH 1.36x10-3
Citric HOOC(OH)C(CH2COOH)2 7.45x10-4 1.73x10-5 4.02x10-7
Crotonic acid (cis) HC4H5O2 3.89 x10-5
Crotonic acid (trans) HC4H5O2 2.04 x10-5
Formic HCOOH 1.80x10-4
Fumaric trans-HOOCCH:CHCOOH 8.85x10-4 3.21x10-5
Glycolic HOCH2COOH 1.47x10-4
Hydrazinium Ion H2NNH3+ 1.05x10-8
Hydrazoic HN3 2.2x10-5
Hydrogen Cyanide HCN 6.2x10-10
Hydrofluoric HF 6.8x10-4
Hydrogen Peroxide H2O2 2.2x10-12
Hydrogen Sulfide H2S 9.6x10-8 1.3x10-14
Hydroxyl Ammonium Ion HONH3+ 1.10x10-6
Hypochlorous HOCl 3.0x10-8
Iodic HIO3 1.7x10-1
Lactic CH3CHOHCOOH 1.38x10-4
Maleic cis-HOOCCH:CHCOOH 1.3x10-2 5.9x10-7
Malic HOOCCHOHCH2COOH 3.48x10-4 8.00x10-6
Malonic HOOCCH2COOH 1.42x10-3 2.01x10-6
Mandelic C6H5CHOHCOOH 4.0x10-4
Methyl Ammonium Ion CH3NH3+ 2.3x10-11
Nitric HNO3 Strong
Nitrous HNO2 7.1x10-4
Oxalic HOOCCOOH 5.60x10-2 5.42x10-5
Periodic H5IO6 2x10-2 5x10-9
Phenol C6H5OH 1.00x10-10
Phosphoric H3PO4 7.11x10-3 6.32x10-8 4.5x10-13
Phosphorous H3PO3 3x10-2 1.62x10-7
o-Phthalic C6H4(COOH)2 1.12x10-3 3.91x10-6
Picric (NO2)3C6H2 OH 4.3x10-1
Piperidinium C5H11NH+ 7.50x10-12
Propanoic CH3CH2COOH 1.34x10-5
Pyridinium C5H5NH+ 5.90x10-6
Salicylic C6H4(OH)COOH 1.06x10-3
Sulfamic H2NSO3H 1.03x10-1
Succinic HOOCCH2CH2COOH 6.21x10-5 2.31x10-6
Sulfuric H2SO4 Strong 1.02x10-2
Sulfurous H2SO3 1.23x10-2 6.16x10-8
Tartaric HOOC(CHOH)2COOH 9.20x10-4 4.31x10-5
Thiocyanic HSCN 0.13
Thiosulfuric H2S2O3 0.3 2.5x10-2
Trichloroacetic Cl3CCOOH 3
Trimethyl Ammonium Ion (CH3)3NH+ 1.58x10-10

115
 Appendix 10

Standard Reduction potential in Aqueous Solution at 25°C

(note the negative potentials are difficult to see here. Ask instructor for clarification.)

Appendix 11
Quantitative Analytical Chemistry, Lab Manual

116
Thermodynamic Quantities for Selected Substances at 298.15 K (25°C)
Modified 8/18
Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Appendix 11 Thermodynamic Quantities for Selected Substances at 298.15 K (25°C)

DHf° DGf° DS° DHf° DGf° DS°
Substance (kJ/mol) (kJ/mol) (J/mol-K) Substance (kJ/mol) (kJ/mol) (J/mol-K)
Aluminum Chlorine
Al (s) 0 0 28.32 Cl (g) 121.7 105.7 165.2
AlCl3 (s) - 705.6 - 630.0 109.3 Cl- (aq) - 167.2 - 131.2 56.5
Al2O3 (s) - 1669.8 1576.5 51.00 Cl2 (g) 0 0 222.96
Barium HCl (aq) - 167.2 - 131.2 56.5
Ba(s) 0 0 63.2 HCl (g) -92.30 -95.27 186.69
BaCO3(s) - 1216.3 - 1137.6 112.1 Chromium
BaO(s) - 553.5 - 525.1 70.42 Cr (g) 397.5 352.6 174.2
Beryllium Cr (s) 0 0 23.6
Be(s) 0 0 9.44 Cr2O3 (s) - 1139.7 - 1058.1 81.2
BeO(s) - 608.4 - 579.1 13.77 Cobalt
Be(OH)2(s) - 905.8 - 817.9 50.21 Co (g) 439 393 179
Bromine Copper
Br(g) 111.8 82.38 174.9 Cu (s) 0 0 33.30
Br-(aq) - 120.9 - 102.8 80.71 CuCl2 (s) - 205.9 - 167.7 108.1
Br2(g) 30.71 3.14 245.3 CuO (s) - 156.1 - 128.3 42.59
Br2(l) 0 0 152.3 Cu2O (s) - 170.7 - 147.9 92.36
HBr(g) -36.23 -53.22 198.49 Fluorine
Calcium F (g) 80.0 61.9 158.7
Ca(g) 179.3 145.5 154.8 F- (aq) - 332.6 - 278.8 - 13.8
Ca(s) 0 0 41.4 F2 (g) 0 0 202.7
CaCO3 (s, calcite) - 1207.1 -1128.76 92.88 HF (g) - 268.61 -270.70 173.51
CaCl2(s) - 795.8 - 7484 104.6 Hydrogen
CaF2(s) - 1219.6 - 1167.3 68.87 H (g) 217.94 203.26 114.60
CaO(s) - 635.5 -604.17 39.75 H+(aq) 0 0 0
Ca(OH)2(s) - 986.2 - 898.5 83.4 H+ (g) 1536.2 1517.0 108.9
CaSO4(s) - 1434.0 - 1321.8 106.7 H2 (g) 0 0 130.58
Carbon Iodine
C(g) 718.4 672.9 158.0 I (g) 106.60 70.16 180.66
C(s, diamond) 1.88 2.84 2.43 I- (aq) -55.19 -51.57 111.3
C(s, graphite) 0 0 5.69 I2 (g) 62.25 19.37 260.57
CCl4 (g) - 106.7 - 64.0 309.4 I2 (s) 0 0 116.73
CCl4 (l) - 139.3 - 68.6 214.4 HI (g) 25.94 1.30 206.3
CF4 (g) - 679.9 - 635.1 262.3 Iron
CH4 (g) - 74.8 - 50.8 186.3 Fe (g) 415.5 369.8 180.5
C2H2 (g) 226.7 209.2 200.8 Fe (s) 0 0 27.15
C2H4 (g) 52.30 68.11 219.4 Fe2+ (aq) -87.86 -84.93 113.4
C2H6 (g) -84.68 -32.89 229.5 Fe3+ (aq) -47.69 -10.54 293.3
C2H5 (g) -103.85 -23.47 269.9 FeCl2 (s) - 341.8 - 302.3 1179
C4H10 (g) -124.73 - 15.0 310.0 FeCl3 (s) - 400 - 334 142.3
C4H10 (l) - 147.6 - 15.0 231.0 FeO (s) - 271.9 - 255.2 60.75
C6H6 (g) 82.9 129.7 269.2 Fe2O3 (s) -822.16 -740.98 89.96
C6H6 (l) 49.0 124.5 172.8 Fe3O4 (s) - 1117.1 - 1014.2 146.4
CH3OH (g) - 201.2 - 161.9 237.6 FeS2 (s) - 171.5 - 160.1 52.92
CH3OH (l) - 238.6 -166.23 126.8 Lead
C2H5OH (g) - 235.1 - 168.5 282.7 Pb (s) 0 0 68.85
C5H5OH (l) - 277.7 -174.76 160.7 PbBr2 (s) - 277.4 - 260.7 161
C6H12O6 (s) -1273.02 - 910.4 212.1 PbCO3 (s) - 6994 - 625.5 131.0
CO (g) - 110.5 - 137.2 197.9 Pb(NO3)2 (aq) -421.3 -246.9 303.3
CO2 (g) - 393.5 - 394.4 213.6 Pb(NO3)2 (s) - 451.9 - -
HC2H3O2 (l) - 487.0 - 392.4 159.8 PbO (s) - 217.3 - 187.9 68.70
Cesium Lithium
Cs (g) 76.50 49.53 175.6 Li (g) 159.3 126.6 138.8
Cs (s) 0 0 85.15 Li (s) 0 0 29.09
CsCl (s) - 442.8 - 414.4 101.2 Li+ (g) 685.7 648.5 133.0
LiCl (s) - 408.3 - 384.0 59.30

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

DHf° DGf° DS° DHf° DGf° DS°

Substance (kJ/mol) (kJ/mol) (J/mol-K) Substance (kJ/mol) (kJ/mol) (J/mol-K)
Magnesium K2O (s) - 363.2 - 322.1 94.14
Mg (g) 147.1 112.5 148.6 KO2 (s) - 284.5 - 240.6 122.5
Mg (s) 0 0 32.51 K2O2 (s) -495.8 -429.8 113.0
MgCl2 (s) - 641.6 - 5924 89.6 KOH (s) - 424.7 - 378.9 78.91
MgO (s) - 601.8 - 569.6 26.8 KOH (aq) - 482.4 - 440.5 91.6
Mg(OH)2 (s) - 924.7 - 833.7 63.24 Rubidium
Manganese Rb (g) 85.8 55.8 170.0
Mn (g) 280.7 238.5 173.6 Rb (s) 0 0 76.78
Mn (s) 0 0 32.0 RbCl (s) - 430.5 - 412.0 92
MnO (s) - 385.2 - 362.9 59.7 RbClO3 (s) - 392.4 - 292.0 152
MnO2 (s) - 519.6 - 464.8 53.14 Scandium
MnO4 - (aq) -541.4 -447.2 191.2 Sc(g) 377.8 336.1 174.7
Mercury Sc(s) 0 0 34.6
Hg (g) 60.83 31.76 174.89 Selenium
Hg (l) 0 0 77.40 H2Se(g) 29.7 15.9 219.0
HgCl2 (s) - 230.4 - 184.0 144.5 Silicon
Hg2Cl2 (s) - 264.9 - 210.5 192.5 Si (g) 368.2 323.9 167.8
Nickel Si (s) 0 0 18.7
Ni (g) 429.7 384.5 182.1 SiC (s) -73.22 -70.85 16.61
Ni (s) 0 0 29.9 SiCl4 (l) - 640.1 - 572.8 239.3
NiCl2 (s) - 305.3 - 259.0 97.65 SiO2 (s, quartz) -910.9 - 856.5 41.84
NiO (s) - 239.7 - 211.7 37.99 Silver
Nitrogen Ag (s) 0 0 42.55
N (g) 472.7 455.5 153.3 Ag+ (aq) 105.90 77.11 73.93
N2 (g) 0 0 191.50 AgCl (s) - 127.0 -109.70 96.11
NH3 (aq) -80.29 -26.50 111.3 Ag2O (s) -31.05 -11.20 121.3
NH3 (g) -46.19 -16.66 192.5 AgNO3 (s) - 124.4 -33.41 140.9
NH4+(aq) - 132.5 - 79.31 113.4 Sodium
N2H4 (g) 95.40 159.4 238.5 Na (g) 107.7 77.3 153.7
NH4CN (s) 0.0 - Na (s) 0 0 51.45
NH4Cl (s) - 314.4 - 203.0 94.6 Na+ (aq) - 240.1 - 261.9 59.0
NH4NO3 (s) - 365.6 - 184.0 151 Na+ (g) 609.3 574.3 148.0
NO (g) 90.37 86.71 210.62 NaBr (aq) -360.6 - 364.7 141
NO2 (g) 33.84 51.84 240.45 NaBr (s) - 361.4 - 349.3 86.82
N2O (g) 81.6 103.59 220.0 Na2CO3 (s) - 1130.9 - 1047.7 136.0
N2O4 (g) 9.66 98.28 304.3 NaCl (aq) - 407.1 - 393.0 115.5
NOCl (g) 52.6 66.3 264 NaCl (g) - 181.4 - 201.3 229.8
HNO3 (aq) - 206.6 - 110.5 146 NaCl (s) -410.9 -384.0 72.33
HNO3 (g) - 134.3 -73.94 266.4 NaHCO3 (s) -947.7 -851.8 102.1
Oxygen NaNO3 (aq) -446.2 -372.4 207
O (g) 247.5 230.1 161.0 NaNO3 (s) - 467.9 - 367.0 116.5
O2 (g) 0 0 205.0 NaOH (aq) -469.6 -419.2 49.8
O3 (g) 142.3 163.4 237.6 NaOH (s) -425.6 - 379.5 64.46
- - 230.0 - 157.3 - 10.7 Strontium
OH (aq)
H2O (g) - 241.82 -228.57 188.83 SrO (s) - 592.0 - 561.9 54.9
H2O (1) -285.83 -237.13 69.91 Sr (g) 164.4 110.0 164.6
H2O2 (g) - 13640 -105.48 232.9 Sulfur
H2O2 (l) - 187.8 - 120.4 109.6 S (s, rhombic) 0 0 31.88
Phosphorus SO2 (g) - 296.9 - 300.4 248.5
P (g) 316.4 280.0 163.2 SO3 (g) - 395.2 - 370.4 256.2
P2 (g) 144.3 103.7 218.1 2- - 909.3 - 744.5 20.1
SO4 (aq)
P4 (g) 58.9 24.4 280 SOCl2 (l) - 245.6 - -
P4 (s, red) -17.46 -12.03 22.85 H2S (g) -20.17 - 33.01 205.6
P4 (s, white) 0 0 41.08 H2SO4 (aq) - 909.3 - 744.5 20.1
PCl3 (g) -288.07 - 269.6 311.7 H2SO4 (l) -814.0 - 689.9 156.1
PCl3 (l) - 319.6 - 272.4 217 Titanium
PF5( g) - 1594.4 - 1520.7 300.8 Ti (g) 468 422 180.3
PH3 ( g) 5.4 13.4 210.2 Ti (s) 0 0 30.76
P4O6 (s) - 1640.1 - - TiCl4 (g) - 763.2 - 726.8 354.9
P4O10 (s) - 2940.1 - 2675.2 228.9 TiCl4 (1) - 804.2 - 728.1 221.9
POCl3 (g) - 542.2 - 502.5 325 TiO2 (s) - 944.7 - 889.4 50.29
POCl3 (l) - 597.0 - 520.9 222 Vanadium
H3PO4 (aq) - 1288.3 - 1142.6 158.2 V (g) 514.2 453.1 182.2
Potassium V (s) 0 0 28.9
K (g) 89.99 61.17 160.2 Zinc
K (s) 0 0 64.67 Zn (g) 130.7 95.2 160.9
KCl (s) - 435.9 -408.3 82.7 Zn (s) 0 0 41.63
KClO3 (s) - 391.2 - 289.9 143.0 ZnCl2 (s) - 415.1 - 369.4 111.5
KClO3 (aq) - 349.5 - 284.9 265.7 ZnO (s) - 348.0 - 318.2 43.9
KNO3 (s) -492.70 -393.13 288.1

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Appendix 12
Logger Pro 3 Quick Reference

Vernier Web site: www.vernier.com

To download a pdf file of this tutorial: http://www2.vernier.com/manuals/LP3QuickRefManual.pdf
Dr. Garces Website Vernier Tutorial:
http://www.miramar.sdccd.net/faculty/fgarces/ChemComon/LabMatters/Vernier/Vernier.htm

Getting Started
Logger Pro Requirements
To use Logger Pro, you must have the following equipment:

Windows 98®, 2000, ME, NT, or XP on a Pentium® processor or equivalent, 133 MHz, 32 MB RAM, 25 MB of
hard disk space, for a minimum installation.
Mac OS® 9.2, or Mac OS X (10.1 or newer), with 25 MB of hard disk space for a minimum installation.

Using the movie feature of Logger Pro will require a faster processor and an additional 100 MB of hard disk
space. Movies are supported by QuickTime®, which you can add during Logger Pro installation.

Note: Logger Pro cannot be used with the ULI or Serial Box interface.

Load Logger Pro

Windows
Place the Logger Pro CD in the CD-ROM drive of your computer.

If you have Auto run enabled, the installation will launch automatically; otherwise choose Settings→Control
Panel from the Start menu. Double-click on Add/Remove Programs. Click on the Install button in the
resulting dialog box.

The Logger Pro installer will launch, and a series of dialog boxes will step you through the installation of
the Logger Pro software. It is recommended that you accept the default directory.

Macintosh
Place the Logger Pro CD in the CD-ROM drive of your computer and double-click on the CD icon.
Double-click the “Install Logger Pro” icon and follow the instructions on the screen.

Get Everything Ready

Using a computer, you will need the following to collect data with Logger Pro:
A free USB or serial port on your computer
A Vernier LabPro® interface:

To collect data, you will need a Vernier LabPro with its power supply and USB
or serial cable (cables provided with LabPro).

At least one sensor:

A Motion Detector or Stainless Steel Temperature Probe are good choices for initial
testing of Logger Pro. The Voltage Probe included with the LabPro interface can also be
used. If available, use a new sensor that supports the auto-ID feature.

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Initial Setup
Before launching Logger Pro, you should:
Power the LabPro using the AC power supply or AA batteries.

Connect a sensor to LabPro.

Connect the USB or serial cable to LabPro.

Attach the other end of the interface cable to any unused serial
port or USB port on your computer.

Start Up Logger Pro

Locate the Logger Pro icon and double-click on it. Mac OS X users can find the icon in the Logger Pro folder
created during installation.

Note: The first time that you run Logger Pro with your LabPro interface, a message may appear notifying you
of an update to the LabPro operating system. You will need to proceed with this update. This may take several
minutes.* The process is significantly faster if you use the USB rather than the serial cable.

* Important: Do not interrupt this update.

If Logger Pro has successfully detected the interface, you will see the LabPro status (see figure below). Also,
if an auto-ID sensor was attached, the current sensor reading will appear below the toolbar (as shown in the
figure).

Nice job! You have successfully set up your equipment and installed Logger Pro. Keep reading for instructions
on the various ways to collect and obtain data. You will also learn how to use Logger Pro’s powerful features,
such as data analysis, movies, and customizing your experiments.

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Appendix 13
Miscellaneous Chemical Information

Conversion | Quantum | Gas Laws | Fpt-Bpt | VSEPR | Solubility | Solution | Colligative |

Equilibrium | Acid-Base | Kinetics | Thermo-Electro | Inorganic | Organic | Periodic Table

Conversion information
System Pressure: LENGTH: VOLUME MASS Temperature
English: 760mmHg = 14.7psi 1 ft = 12 in 1 gal = 4 qt 1 lb = 16 oz
T  = 1.8T  + 32
1 atm = 101.3 KPa 1 mile = 5280 ft 32oz = 1 qt 1 ton = 2000lb F C

1 qt = 57.75 in3
SI- 1 atm = 760 torr 1 in = 2.54 cm 1 L = 1.057 qt 1 lb = 453.6 g (T  − 32)
English: 1atm = 760 mmHg 1 mi = 1.609 km 1 qt = 0.946 L 1 oz = 28.35 g T = F
C
1.8
Misc. info 1 J = 1 kg m2 / s2 1 mole = 6.02•1023 Density H2O: 1.0 g/mL

Quantum Equations
Electromagnetic hc , h = 6.63 • 10 -34 J•s , c = 3.0 •108 m/s
Radiation E = h •ν =
λ
Energy for ! 1 $
H-like atom E =Z2 Rh # &
#" n 2 &%
Rydberg Equation " % ! $
1 1 ' 1 1 1 &
ΔE = R H $ - = R H (λ ) # -
$n2 nf2 '& "ni nf2 &%
# 2
# i λ
RH(E) = 2.18 • 10-18 J RH (l) = 1.097 • 107 m-1

Gas law equations

Ideal Gas Law
PV = nRT m • P L • atm
Denstiy(D) = , m= mass R = 0.08206
n RT mol • K
Real Gas ! a • n2 $
Vander Waal Equation # P+
#
" V2 %
& (
& V-n • b = nRT )
STP
P = 1 atm, T = 0°C, 1mole = 22.4 L
Dalton's Law
(n a +n b +n c +...)R • T
of Partial Pressure PT = Pa + Pb + Pc + ... PT = .
VT
Pa = ca • PT Pb = cb • PT .ca = na / nT cb = nb / nT
Speed of Gas particles
1 3RT J
KE= mu2 u rms = R = 8.314
2 M mol • K
Graham's Law of
rate a time b Mb
effusion = =
rate b time a Ma
Calorimetry qp = DH = m Cs DT where DT = Tf - Ti, Cs (H2O) = 4.184 J/g•K

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Valence Shell Electron-Pair Repulsion Theory (VSEPR)

e- AEn Electronic Geometry Bond Lone - AEnBm Molecular Geometry Bond angle Examples
Domain atoms pairs Hybrid

2 AE2
E A E 2 0 AB2 B A B 180°
sp
BeH2

Linear Linear CO2

E 3 0 AB3 B 120° BF3

B A
A BCl3
3 AE3 E E B Trigonal sp2
Trigonal 2 1 AB2E B < 120° NO2
A

..
B Bent sp2
4 0 AB4 B 109.5° CH4

A NH4+
B sp3
B
E B Tetrahedral
3 1 AB3E .. < 109.5° NH3
4
E A E A
AE4 E
B B sp3
Tetrahedral B Pyramidal
2 2 AB2E2 .. < 109.5° H2O

.. A
B sp3
B Bent
5 0 AB5 B 180° P I5
B 120°
B A 90°
B
E B Trig Bipyramidal sp3d
E 4 1 AB4E B 180° S F4
E A E 90°
E B
A
..

<120°

5 AE5
B
Trig Bipyramidal B See-saw sp3d
3 2 AB3E2 B 180° Cl F3
B 90°
A
..

..

B T-shape sp3d
2 3 AB2E3 B 180° Xe F2
..

A
..

sp3d
..

B Linear
6 0 AB6 B 90° S F6
B B
A
B B
E sp3d2
E
B Octahedral
E
..
E A E 5 1 AB5E 90° Br F5
6 AE6 E B
A
B < 90°
B B
Octahedral
B Square Pyramidal sp3d2
4 2 AB4E2 .. 90° Xe F4
B B
A
B B
sp3d2
..
Square planar

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Boiling Points of Liquids

Liquid Boiling Point
(°C)
1 Acetone 56.5
2 Carbon disulfide 46.3
3 Carbon tetrachloride 76.8
4 Chloroform 61.3
5 Ethanol 78.5
6 Ether 34.6
7 Methanol 64.6
8 Water 100.0

Solubility rules
Soluble substances with - Exceptions Insoluble substances with - Exceptions

(NO3-) (ClO3-) (S2-), (CO32- ), Grp1A, NH4+

None
(ClO4-) (CH3COO-) (CrO42-), (PO43-)

X- = Cl-, Br-, I- Ag, Hg, Pb (OH-) Grp1A, NH4+, Sr, Ba, Ca

(SO42-) Sr, Ca, Ba, Hg, Pb Soluble - dissolve, no precipitate (aq -phase)

Alkali & NH4+ None insoluble (or slightly soluble) - does not dissolve,
precipitate forms. (s-phase)

Solubility Table
C2H3O2- AsO4 3- Br - CO3 2- Cl - CrO4 2- OH - -
I - NO3 C2O4
2- 2- PO 3-
O 4 SO42- S 2- SO3
2-

Al+3 S I S - S - I S S - I I S d -

NH4+ S S S S S S S S S S S S S S S

Ba2+ S I S I S I s S S I s S S S S

Bi3+ - s d I d - I I d I I s d I -

Ca2+ S I S I S S I S S I I I I d I

Co2+ S I S I S I I S S I I I S I I

Cu2+ S I S I S I I - S I I I S I -

Fe2+ S I S s S - I S S I I I S I s

Fe3+ I I S I S - I - S S I I S I -

Pb2+ S I I I I I I I S I I I I I I

Mg2+ S d S I S S I S S I I I S d s

Hg2+ S I I I S s I I S I I I d I -

K+ S S S S S S S S S S S S S S S

Ag+ s I I I I I - I S I I I I I I

Na+ S S S S S S S S S S S S S S S

Zn 2+ S I S I S I I S S I I I S I I
S = Soluble in water I = Insoluble in water (lessthan 1 g./100 g H2O) s = slightly soluble in water d = Decomposes in water

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Solution and Concentration equations:

Concentrations
Solution Dilution
M, molarity = moles solute / liter solution
N , normality = eq solute / liter solution
m , molality = moles solute / Kg solvent
% m, percent by mass = (mass solute / mass solution)*100
c , mole fraction = moles a / moles a + moles b ...
C1V1 = C2V2 (moles before dilution = moles after dilution)

Solubility and Colligative Properties

Pressure effects; Henry's Law P = c/k where c = solubility
Raoult's Law Psolv = P csolvent • P°solvent
DPsolv = P°solv - Psolv = Psolute • P°solv
Boiling Point Elevation DTb = m Kb
Freezing Point Depression DTf = m Kf
Osmotic Pressure P = MRT (R = 0.08206 L•atm / mol•K)
Van't Hoff Factor i moles particles solution (expt)
i=
moles solute dissolved (calculated conc)

Equilibrium
Equilibrium constant Kp & Kc Kp = Kc(RT)Dn Kc = Kp(RT)-Dn
Quadratic Eqn : ax2 + bx + c = 0 −b ± b2 − 4ac
x=
2a

Acid Base
pX and [X] Relationship pH = -log [H3O+] pOH = -log [OH-] pKa = -log [Ka]
[H3O+]= 10-pH [OH-]= 10-pOH [Ka]= 10-pKa
Kw Kw = 1•10-14 @ 25°C Kw = Ka•Kb 14 = pH + pOH
Henderson - Hasselbalch pH = pKa + log [Cb/Ca] pOH = pKb + log [Ca/Cb]
Equation

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Kinetics
Rates of Reaction Rate = D[A] /D t = - D [react] /D t = D [prod] /Dt
Rate laws (Order of Initial rate = k [A]x [B]y [C]z Overall order = x + y + z + ...
reaction) ...

Conc. vs. Time Graph Relationship

Equations
dependence
Zeroth Order [A] = [A]o - kt Conc. vs. Time c straight line.
rate = k
Half life; t1/2 = [A]o / 2 k

First Order [A]= [A]o exp {- kt) Ln[Conc.] vs. Time c straight line
rate = k [A]
Ln[A] = Ln[A]o - kt Half life; t1/2 = 0.693 / k

Second Order 1/[A] = 1/[A]o + kt 1/[Conc.] vs. Time c straight line

rate = k [A]2 Half life; t1/2 = 1 / k [A]o
or k [A] [B]
k= A exp {-Ea /RT}
Temperature vs. Rate
Ln(k) = Ln(A) - (Ea/R)•1/T Ln(k) vs. 1/T c straight line.
dependence

ThermoDynamics - Electrochemistry
Thermodynamics Cell Potential, DG and Keq
Standard Conditions: 1 atm, 25°C DG = - nFE
DG° = - nFE°
Universe = surroundings + system E° = (0.05916 / n ) log Keq
State Function (X) where X = E, H, S or G
E°cell = E°red(cathode) - E°red(anode)
DXrxn = S n DX°prod - S n DX°react
E°cell = E°red + E°ox
w = -P DV
DE = q + w
Cell concentration and the Nernst equation
DH = DE + P DV
E° = (RT/ nF) Ln(Keq)
DH = qp
E° = (0.05916/ n) log(Keq)
DS°univ = DS°surr + DS°sys
E = E° - (0.05916 / n) log(Q)
DS°surr = - DH°sys / T
DG = DH - TDS
2H2O (l) + 2e- g H2 (g) + 2OH- (aq)
DG = DG° + RT Ln(Q)
E° = - 0.83 V
DG° = - RT Ln(Keq)
O2(g) + 4H+ (aq) + 2e- g 2H2O (l) E° = +1.23V

Keq = exp {-DG° /RT}

Constants
Ln(Keq) = (DS°/ R) - (DH°/ RT)
R = 8.314 J / mol•K
F = 96,485 C / mol e-

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Quantitative Analytical Chemistry, Lab Manual Modified 8/18

Inorganic
Spectro-chemical Series:
I-- < Br- < Cl- < NO3- < F- < CO32- < OH- < C2O42- < H2O < NH3 = en < NO2- < phen < bpy < SCN- < CN- < CO < ppy-
f Weak Field Ligands Strong Field Ligands g
Bidentate Ligands

phen bpy ppy -

Abbreviation
Ox2- (oxalato), en (ethylenediamine), phen (1,10-phenathroline),
ppy – (2-phenylpyridine), bpy (2,2’-bipyridine),
EDTA (ethylenediaminetetraacetate)

Color Wheel

Organic: Nomenclature

126
 Quantitative Analytical Chemistry, Lab Manual Modified 8/18

1 18
IA VIIIA
1 1 2
H 2 13 14 15 16 17 He
1.00797 IIA IIIA IVA VA VIA VIIA 4.0026

2 3 4 5 6 7 8 9 10
Li Be B C N O F Ne
6.939 9.0122 10.811 12.0112 14.0067 15.9994 18.9984 20.179

3 11 12 13 14 15 16 17 18
Na Mg 3 4 5 6 7 8 9 10 11 12 Al Si P S Cl Ar
22.9898 24.305 IIIB IVB VB VIB VIIB VIIIB IB IIB 26.9815 28.086 30.9738 32.064 35.453 39.948

4 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
39.102 40.08 44.956 47.90 50.942 51.996 54.9380 55.847 58.9332 58.71 63.54 65.37 65.37 72.59 74.9216 78.96 79.909 83.80

5 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
85.47 87.62 88.905 91.22 92.906 95.94 [99] 101.07 102.905 106.4 107.870 112.40 114.82 118.69 121.75 127.60 126.904 131.30

6 55 56 57 * 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86
Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
132.905 137.34 138.91 178.49 180.948 183.85 186.2 190.2 192.2 195.09 197.0 200.59 204.37 207.19 208.980 [210] [210] [222]

7 87 88 89 ‡ 104 105 106 107 108 109 110 111 112

Fr Ra Ac Rf Db Sg Bh Hs Mt
[269] [272] [277]
[223] [226] [227] [261] [262] [263] [262] [265] [266]

* Lanthanide 58 59 60 61 62 63 64 65 66 67 68 69 70 71
Series Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
140.115 140.9077 144.24 (145) 150.368 151.965 157.25 158.9254 162.50 164.9303 167.26 168.9342 173.04 174.967

‡ Actinide 90 91 92 93 94 95 96 97 98 99 100 101 102 103

Series Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
232.0381 231.0359 238.0289 237.048 [244] [260] [247] [247] [251] [252] [257] [258] [259] [260]

Links to Periodic Table on the Web:

1. http://www.webelements.com/
2. http://pearl1.lanl.gov/periodic/default.htm
3. http://www.chemicalelements.com/
4. http://chemlab.pc.maricopa.edu/periodic/periodic.html
5. http://www.chemsoc.org/viselements/

Useful Chemistry Links

1. Vernier Download Page: http://www.vernier.com/downloads/index.html

127