Chem 223: Experiment 1

GENERAL INFORMATION

(This experiment is completely follows the lab. “General information”. Chem 223. UIUC)

PRINT OUT THE FORM ON THE NEXT PAGE.

READ IT.
READ IT AGAIN.
If you understand it, sign it and bring it to turn in to your instructors at the first lab.
If there is anything you do not understand, bring the UNSIGNED form to the first lab, ask the
instructor to clarify anything that you do not understand, then sign it and turn it in.
KEEP A SIGNED COPY OF THE FORM
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 I. Chemistry Laboratory Regulations

General Regulations. The following rules, designed to preserve your health, will be strictly
enforced.

1. Eye protection must be worn at all times in the laboratory. Regular glasses do not provide
sufficient protection and therefore safety goggles will be required. Never wear contact lenses in
the lab; vapors can be trapped behind the lens and cause irreparable corneal damage. Safety
goggles are available for purchase at safety- work shops. If you are caught just once not
wearing proper protective eyewear in lab, you will be dismissed for the day, and miss finishing
that lab. If you are caught twice, you will be dismissed from the lab for the remainder of the
course.
2. No one is allowed in the laboratory at any time without proper supervision; i.e., a qualified lab
assistant or faculty member must be present.
3. No smoking, food, or beverages are allowed in the laboratory.
4. Shoes must be worn in the lab at all times. Sandals are not allowed because they do not provide
sufficient protection from falling equipment and chemicals.
5. Secure long hair behind the head to prevent it from coming near moving equipment or burners.
6. Your clothes must cover the trunk of your body and your shoulders. A lab apron or coat is also
required and available for purchase at workplace safety shops.

Safety Precautions.
1. Know the location and use of the fire extinguishers, fire blanket, eyewash, safety shower, and
first aid kit.
2. Be careful about smelling chemicals; avoid breathing any vapors. Work in a ventilation hood
when carrying out reactions involving volatile substances or gases. If you must determine the
odor of a compound, fan the vapors towards your nose, and sniff cautiously. Do not taste any
compounds; some are toxic or contain toxic impurities. Avoid prolonged exposure (inhalation
or absorption through the skin) of organic compounds. Common organic solvents such as
acetone, methanol, chloroform, carbon tetrachloride, benzene, aniline, nitrobenzene, phenol,
etc. are toxic. Use the hood when possible.
3. When heating a container such as a test tube, do not point the mouth of the container at your
neighbors or yourself. The liquid may suddenly boil or bump, causing the liquid to be blown
out of the mouth of the container.
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4. Always make sure that the apparatus set-up used in an experiment does not involve a closed
system. For example, be certain that you have made provisions for the escape of air as your
equipment is heated.
5. Never pour water into concentrated acid. Always pour the acid slowly into the water with
constant stirring. Large amounts of heat are released when an acid, such as sulfuric acid,
undergoes hydration. Under certain conditions, steam is generated, blowing acidic vapor from
the container.
6. Avoid the use of strong oxidizing agents with organic compounds when cleaning glassware.
The combination of organic residue and nitric acid can be explosive.
7. Most laboratory accidents are lacerations caused by a failure to observe simple precautions
when handling glassware. Always protect your hand with a towel when cutting glass tubing or
inserting it into a stopper. When inserting glass tubing into a stopper, always lubricate the
tubing with glycerol so that it will pass easily through the stopper. Glycerol is available at the
reagent shelf or in the stockroom.
8. If you have an accident, obtain help by notifying the person in charge immediately.
9. Absolutely no pipetting by mouth; use a rubber bulb.

I have read the above regulations and safety precautions, discussed them with the professor
or TA, and retained the following copy for my own reference. Sign this copy and turn in.
Date__________ Signed __________________Print Name ____________________

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 II. Books on Reserve

- Brewer, S. Solving Problems in Analytical Chemistry.

- Christian, G.D. Analytical Chemistry, 6th ed., 2004
- Fritz, J.S. and D.M. Schenk, Jr. Quantitative Analytical Chemistry, 4th ed.
(especially pp. 582 & 621)
- Harris, D.C. Quantitative Chemical Analysis, 7th ed., 2007.
- Laitinen, H.A. and W.E. Harris,. Chemical Analysis, 2nd ed.
- Ramette, R.W. Chemical Equilibrium and Analysis
- Skoog, D.A. and D.M. West. Analytical Chemistry, 4th ed.
- Skoog, D.A., D.M. West, and F.J. Holler. Fundamentals of Analytical Chemistry, 5th ed.
- David Harvey. Modern analytical chemistry, 2000.
- D. Kealey & P.J. Haines. Analytical chemistry ( Instant notes). 2002

References for lab experiments cited at the beginning of most labs in this manual refer to the
following sources, which you may find helpful.

C = G. D. Christian, Analytical Chemistry, 6th Ed., John Wiley & Sons, 2004.
H7 = D. C. Harris, Quantitative Chemical Analysis, 7th ed., W. H. Freeman& Co., 2007.
S & W = D. A. Skoog and D. M. West, Analytical Chemistry, 4th Ed., Holt, Rinehart, and
Winston, Inc., 1986.
SWH = D. A. Skoog, D. M. West, F. J. Holler, Fundamentals of Analytical Chemistry, 5th
Ed.,Saunders College Publishing, 1988.
Harvey= David Harvey. Modern analytical chemistry,Mac Graw Hill 2000.
Kealey= D. Kealey & P.J. Haines. Analytical chemistry (Instant notes).BIOS Scienific
Publisher. 2002

III. General Laboratory Directions

The general purpose of this laboratory is to promote proficiency and familiarity with the
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techniques of chemical analysis, especially with their particular abilities for solving real
problems and shortcomings. While the problems and methods are those of classical wet
chemistry, augmented with chromatography and spectrophotometry, the approaches of
equilibrium, kinetics, and stoichiometry are general for all chemical analyses. In lab, you will
have "hands-on" experience with a number of specific analyses. These have been selected
with 3 goals in mind:

1. Workability - you should be able to succeed.

2. Utility - These are real techniques that are frequently performed in working analytical
laboratories - for example, in clinical or agricultural, metallurgical labs... While you
may never perform another titration after you finish quant., you may well have
occasion to submit samples for analysis. The experience you gain in this course should
let you know what to expect from such an analysis - and what not to expect.
3. Representative - The 13 experiments you will do are certainly not exhaustively
representative of the techniques of analytical chemistry. However the concepts
introduced, and the kind of thinking required, are common to all analytical techniques.
It will be necessary for you to consider what interferes with a particular analysis, and
what steps may be taken to avoid interferences.

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 The laboratory in conjunction with the lectures, should provide a good general feeling for the
terms "accuracy" and "precision." It is important to know ahead of time what accuracy and
precision are needed for an analysis, and then select a technique - or devise one, if necessary -
- which is appropriate.

An analyst's time in industry is charged out at something like $100 an hour (that's not the
salary, unfortunately). A company would quickly lose patience with an analyst or a researcher
who does not know - almost intuitively - how much analysis is needed, and what kind! It is
hoped that you will develop some of that kind of intuition as you move through the course.

Because this kind of understanding is an important goal of this course, you should probably
expect that it will take more than extensive memorization to "ace" the course. If you do the
memorization and do a respectable job in the lab, you will probably get by just fine. However,
you will take little except your grade with you when you finish. On the other hand, if you put
forth the little extra effort necessary to understand the material, you will leave with a better
idea of how to approach problems, not only of analysis, but also of research in general.
Besides, if you understand the material, you will find you need to memorize less.

The heart of quantitative technique is to carry a sample through one or more physical and
chemical manipulations without loss of the sample or introduction of foreign materials.
Ultimately, quantitative means absolutely none of the sample is lost and no foreign material is
added. In line with this, the student must quickly develop independent judgment of his or her
work and common-sense awareness of danger spots that can cause the analysis to go astray. A
thorough knowledge of what you are doing makes this an easy task.

The following is a brief list of information to make you a better analyst.

III.A. Laboratory Safety. If you are not careful in lab, you can get hurt. Common sense and
knowledge combine to make the chances for an accident to occur very slight, but they can still
occur. At the beginning of this lab manual is a page of "Chemistry Laboratory Regulations"
which must be followed. All students will be required to sign a copy of that form to indicate
that they are familiar with and will adhere to these safety regulations.
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THINK BEFORE YOU ACT

III.B. Planning and Efficiency. It is imperative that your lab work be planned ahead of time.
There is sufficient time for each experiment, but without some semblance of order and
thorough knowledge of what you are doing you will not have enough time.

1. Read the experiment and all reference materials before coming to lab.

2. Outline the experimental procedure in your notebook before coming to lab (see the
section concerning the lab notebook).

3. Make good use of your time. When you are waiting for something to dry in the oven, or
digesting something, or waiting for something to cool, etc., start on or prepare for the
next task or experiment. Learn to do more than one thing at a time.

4. Listen for announcements from the TA. Frequently check the chalkboard and bulletin
board.

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 5. Do not be afraid to ask the TAs questions about the experiment. They are there to help
you. At the same time, you should be prepared for them to come around and ask you
questions about the experiment or your technique. All TAs maintain office hours to help
with questions.

6. Label all solutions and label your weighing bottles so you do not get confused. Do not
rely on your memory. Before putting anything in the oven to dry, make sure it is clearly
labeled (don't use labeling tape) with your name and desk #.

7. There are three ovens in the lab. Each one has a different opening time. Open the ovens
only at the designated times. This is so that the ovens can maintain the desired
temperature for the required time.

8. EVERYONE OUT OF LAB BY 5:30 P.M. This means you have to stop your
experiment and clean up by 5:20 P.M., at the latest.

9. Many of the experiments require preparation during the preceding lab; thus, you should
always be at least one experiment ahead of the lab in your reading.

III.C. Neatness and Cleanliness

1. The student who is scrupulously neat and tidy usually does not mix up samples or
reagents, or spill or break or misplace items or information. Cleanliness prevents
accidents and the introduction of foreign material into your sample.

2. Glassware is clean not simply when it appears clean, but when de-ionized water drains
from the vessel as a thin, continuous film, and leaves no droplets behind (especially
the burette and pipettes). A few parts per thousand (or even parts per million) of an
impurity introduced from dirty glassware can significantly affect an analysis. In this
course, that means it may affect your grade. In the real world, it could result in an
incorrect medical diagnosis, or an incorrect forensic result. "Kitchen clean" is not good
enough for the quantitative analysis lab!
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3. Do not over clean your glassware. Soluble salts can be removed with water. Soap and
cleaning solutions are for removing grease and dirt. Rinse everything well with tap water
and a couple of times with de-ionized water.

4. Do not use soap on fritted glass crucibles.

5. Do not use grease on Teflon burette stopcocks.

III.D. Laboratory Manipulations and Equipment

1. Make sure de-ionized water used to make primary standard solutions is at about 20 C.
Hot or cold water will cause an error in the actual volume your volumetric hold.
They're calibrated for 20 C solutions.

2. Do not leave tops off of desiccators. Though desiccator tops can seem difficult to
remove, when carrying a desiccator to the balance room these tops can tumble to the
floor as though they possessed some spark of life. Hold onto the top as well as the
bottom when carrying the desiccator. The desiccator lid (whether being removed or

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 replaced) is properly moved by sliding, rather than lifting. An airtight seal is achieved
by slight rotation and direct downward pressure on the lid.

3. A volumetric flask must be clean, but need not be dry, before use. After introducing the
solute, fill the flask about half full of solvent and mix well. Add additional solvent to
bring the liquid level almost to the mark and mix again. Use a small pipette or a squirt
bottle to add solvent to the line. If you go past the mark, start over. Stopper the flask
and invert a few times to mix. For long-term storage, cover the stopper with Parafilm.

4. To rinse a burette, close the stopcock and add 5-10 mL of solution. Rotate the burette so
the entire inside is rinsed by the solution, then drain through the tip. Repeat two more
times. Fill the burette above the zero mark. Be certain no bubbles are in the tip of the
burette; they can be removed by briefly opening the stopcock.

5. An aqueous solution in a properly cleaned burette or pipette forms a concave surface

called a meniscus. The position of the bottom of the meniscus is taken as the point of
reference when using volumetric glassware. To correctly judge the volume, your eye
must be level with the meniscus, or a parallax error will occur. When reading burettes, it
is convenient to hold a dark card behind the gradation, touching the burette immediately
below the meniscus.

6. Volume increments smaller than a normal drop (which is about 50 L = 0.05 mL, so 20
dr = 1 mL) may be added from a burette. Open the stopcock slightly and allow a small
volume of liquid to form on the tip. Touch the tip to the wall of the titration vessel.
Combine the droplet with the bulk of solution either by rinsing the wall with solvent or
by tipping the titration vessel.

III.E. Reagents.
Reagents used in a quantitative laboratory are generally of high purity and are of utmost
importance in producing good results. Reagents left to the use of several individuals have a
good chance of becoming contaminated, so each of you has a responsibility to see that they do
not.
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1. Always check reagent bottles for formula weights and purity when using them for
standards.

2. Take only what you need.

3. DON'T PUT ANYTHING INTO A REAGENT BOTTLE. Dump out the quantity
you need into a clean container. Then remove from this the quantity desired and properly
dispose of the rest. This means that you may not use a spatula to remove reagent from
the reagent bottle.

4. NEVER PUT ANY REMOVED REAGENT BACK INTO THE REAGENT BOTTLE.

5. A good procedure to accurately weigh solid reagent is to weigh by difference. Place an

amount of the solid reagent that is greater than needed into a clean dry container (beaker
or weighing bottle); weigh accurately. Pour some of the reagent into a second clean dry
container. Weigh the original container a second time. The difference between the first
and second weighings gives accurately the amount transferred to the second container.
Think about this carefully. You'll practice this in the Basic Techniques lab.

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 6. Certain chemicals must be disposed of in special containers and not down the sink.
Follow these instructions when they occur. Keeping heavy metals, strong acids, and
strong bases out of our waste stream is good citizenship and environmentalism in action.

III.F. Instruments.

1. We will use instruments such as balances, pH meters, gas chromatographs, and

spectrometers. These are complex and often delicate. They should be "tinkered" with
only by those people who have an intimate familiarity with the instruments. Please use
them only as instructed. If repair or adjustment is needed, ask the TA.
2. It is also very important to realize that the data you obtain from these instruments are not
sacred; you must know the limitations and advantages of using a particular instrument.

3. Anyone caught mistreating an instrument will be dismissed from the lab.

4. Do not turn knobs to find out what they do.

5. Never change settings on ovens. Check with the TA if something appears amiss.

6. CLEAN UP ALL WEIGHING PAPER AND SPILLED REAGENT BEFORE

LEAVING THE BALANCE AREA.

III. G. Laboratory Notebook.

1. Your notebook is the only good record you have of your performance in lab.

2. You must use a bound notebook (the binding is permanently glued or stitched). This is
how it's done in industry. Loose pages, three ring notebooks, or spiral notebooks are
not acceptable. We recommend an 8.5 x 11 inch notebook with graph paper pages.

3. Your lab notebook should be neat enough that someone else can easily read and
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understand it. Use plenty of room. If you cannot write legibly, then print. If you have
some physical constraint that prevents legible writing, consult your TA. \

4. Your lab notebook should have numbered pages. The first four pages should be an up-to-
date table of contents so any given experiment can be found quickly.

5. All data obtained in the laboratory should be recorded directly in the notebook at the
time the data are obtained. Recording data on loose slips of paper is forbidden. TAs are
authorized to destroy such stray papers.

6. Entries must be made in ink. A mistake is not erased, but crossed out with one line so as
to be still legible, and the correct value written above.

7. After recording a reading in your lab notebook (such as an analytical balance reading, or
a burette reading), go back and double check the reading. Check especially for gross
errors (such as 48.91 mL instead of 47.91 mL).

8. Format for Lab Notebook:

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 a. Reserve pages 1-4 of the notebook for a Table of Contents. It is a good idea to leave
space in the Table of Contents for analytical results for quick reference later.

b. Beginning at the top of Page 5, start Experiment 1

c. For each experiment, begin at the top of a new page. Include:

I. Title, date experiment was begun, and date finished.

II. A brief (3 to 4 sentence) statement of introduction, purpose, and principles upon

which the analysis is based. Relevant balanced chemical equations should also
appear here.

III. Outline of the procedure to be followed.

IV. A neat and complete listing of data taken during the course of the analysis, properly
labeled and identified, presented in a logical order. Remember, someone else will
read these data and you may need it for future calculations, so keep it neat, logical,
and clearly presented. You will find tabular form is best; it is strongly
recommended.

V. Observations you make during the course of the experiment (color changes,
modification of procedure, any observed errors. such as titrating past the
endpoint).

VI. This section will include calculations and results for each sample run. It is your
responsibility (and will be to your advantage) to present results so a minimum of
effort is required to locate them (underline or enclose results in boxes). Finally,
report the mean value for the quantity of interest in the analysis, and the precision
(standard deviation) of the analytical results.
Remember significant figures.
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9. Use only the right-hand pages of the lab notebook; this allows for a neater presentation
and for additions and corrections at a later date as needed on the facing blank pages.

10. Footnote any references that you used to answer questions, or for error analysis or
optional comments.

11. Sections I, II, and III above must be completed before beginning the analysis, and
Section IV must be complete except for the actual experimental data. This will prove
useful for your understanding of the work to be done and help save time while doing the
actual experiments.

12. The TA must initial your notebook on the appropriate page before you can pick
up an unknown. Your notebook will be checked to see if you are prepared for the given
experiment. You may also be asked a question to see if you are prepared. If your
notebook is not completed through the procedure outline, you will not be allowed to
proceed with the experiment.

13. Neatness and logical presentation are a must; if the TA cannot follow your work, the
grade you receive will reflect this. The TA may periodically look at your notebook and
make comments on its appearance.
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 14. An Example of a Procedural Outline

Gravimetric Determination of Chloride.

1. Sample preparation
a) Dry Cl unknown for 2 hours at 110ºC
b) Dissolve 3 carefully weighed Cl samples in 100-150 mL H2O + 1 mL HNO3
2. Procedure
a) Ppt. Cl as AgCl(s) by adding excess AgNO3
b) Heat, stir, and test for completeness of ppt
c) Cool solution to shift chemical equilibrium to right:

Ag+ + Cl- = AgCl(s)

3. Separation Procedure
a) Filter supernatant liquid through glass crucible
b) Wash ppt with dilute HNO3 and pour washes through crucible
c) Quantitatively transfer ppt to crucible

4. Final Prep
a) Dry crucible and ppt in oven for 1-2 hours at 110-120ºC. Cool in desiccator
b) Weigh and repeat (a) until constant weight

III.H. Lab Reports. The report you submit must be on the standard forms and be neat,
legible, and intelligible. If the report cannot be read, it will not be graded. Please read your
report before you submit it (better yet, get someone else to evaluate it); if your statements
make no sense to you they will make no sense to the TA.

Organizational Summary

I. Title of Experiment
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II. Introduction
A short paragraph describing the purpose and principles of the experiment, including
relevant balanced chemical equations.

III. Data and Observations

Standardization data, sample data, or other. Include everything: drying time and
temperature, cooling time, reagent amounts, etc. Necessary data should be taken
from your lab book (immediately following procedural outline).

IV. Calculations and Results

1) For each calculation required in analysis of replicate data sets, one example should
be worked out in detail showing a listing of relationships used and one fully worked
calculation (including appropriate units). Only the results of calculations need be
shown for other samples (i.e., for the second and third samples in a triplicate
analysis).

2) Report the results of the calculations in the units requested. Always report the
mean, the standard deviation, and the confidence interval for your trials.

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 3) Include "FOR YOUR REPORT" items from each experiment.

Lab reports are always due at the beginning of the next lab, one week after the
experiment is completed.
Late work is not accepted.

Graded reports are returned one week after you turn them in. Nota bene: on occasion,
TAs have fallen behind in grading reports. If you don't advise the professor that grading
isn't being done in a timely manner, he or she has no way to know that you aren't getting
timely feedback. Just as we expect students to diligently perform lab work, we expect
TAs to diligently do their jobs. Complaining to your neighbor can't change anything.
Advising the faculty member in charge of the lab as to what is or isn't happening can
have useful results.
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