A General Chemistry Laboratory Manual

The
Rediscovery
Book

CHM 201 and 207

Fall 2022
PART ONE: How to Be Successful in Lab Work

Being successful in the lab is not a matter of exceptional dexterity. If you can handle a
knife and fork, you can obtain good results. The trick in doing lab work is to learn a
particular routine for each basic operation and practice it until it becomes habitual. For
example, in this manual you will find a method for measuring the mass of solids. This
method has been chosen because it is especially foolproof. If you always use it you will
never have any trouble obtaining the mass of a solid and, in time, any other method will
seem strange.

If dexterity is not important, what does matter? Primarily, it is important to understand

what is happening. In any lab, it is tempting to use a "cook-book" approach, but a
student who understands the underlying principles has a profound advantage. He or
she will be able to evaluate the results as they appear, will know when short cuts are
desirable (or fatal) and will have quiet self-confidence, instead of a sense of impending
disaster.

The Role of Measurement in Lab Work

Measurements are made in this course to answer molecular questions. Molecules can
be investigated only indirectly by finding observable information that can be directly
related to the quantity being measured. You never really look at molecules; rather, you
look at meter readings and try to interpret them.

In such an inquiry, it is easy to measure something other than what you expect to
measure, a situation known as systematic error. A major source of systematic error is
various sorts of instrument malfunctions. To guard against this, there are a number of
very quick proof-of-method experiments in the text. These require almost no
calculation, and if the proof-of-method experiment works, you can be reasonably sure
that the method will actually produce "real” results, unaffected by instrument
problems. This approach is constantly used in scientific research.

Another source of systematic error is failure to control important variables. If you wish
to know the boiling point of a liquid, the atmospheric pressure is a significant variable.
Usually, it is possible to use controls or blanks to avoid these problems. It is sometimes

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possible to compensate for these variables if you have remembered to measure them,
but it is essential to think about them when planning the experiment.
Besides recording experimental results, you should record variables that are controlled
by the experimenter. It may or may not be important to know the concentration of a
solution, for example. One of the reasons for the many repetitions of experiments in
real research is to weed out the various possible systematic errors, until the result can be
stated confidently. In this course, much of this work has been done, but it is still
important to consider how changes in procedure might affect the result.

The Laboratory Notebook - Keeping Records

Nowhere is habit so important as in keeping accurate records. A number of otherwise

inexplicable student results are caused by scrambled records, and studies of laboratory
exams have shown that this is a major cause of student failure. Therefore, most teachers
are strict about notebooks - this is an attempt to save students from themselves.

Your notebook must be:

- Of the approved type, and have tear out copy pages.
- Data must be recorded in ink.
- It must be current and consecutive, and all your work must be in one place.
- Record everything that is relevant at the time you make the measurement.
- Take your notebook everywhere. Never write anything related to the
experiment on scrap paper, your hand, etc.
- Never, never tear out pages (except copy pages): not if you make a mistake, not
if you spill something, never!

Record three classes of data.

1. All of the numbers pertaining to the experiment. Identify all numbers and follow by a
unit. Be sure to record concentrations of stock solutions. Remember, this information
must be recorded directly in your notebook. Even if it is transferred once, there is a
danger of, for example, digits being interchanged, so be sure to take your notebook
everywhere you go.

2. All the observations you have made. This includes smells, colors, and color changes. It
includes the size and shape of solid crystals, abrupt changes in temperature, or any
other phenomena. When in doubt, record it.

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3. Any changes in procedure. If you diluted a reagent down from a concentrated stock
solution, record it. If there was a dead fly in your flask when you did a titration, record
it. When in doubt, record it. You may be tested on the facts you have observed. You
will be permitted to have your notebook for reference during the lab exams, so it will be
to your advantage if it is complete and readable.

In some colleges, at the end of each period you must turn in a carbon copy of your
notebook for that period. This is not only to keep you honest; it helps you if your
notebook is lost or stolen, because it serves as a record.

A good notebook will state everything that was done, and what you observed during
the experiment. Good records will allow you or anyone to know how to repeat the
experiment.

Getting Ready for Lab

Read the experiment carefully from beginning to end. (Check the schedule to see that
you are preparing for the correct experiment!) Ask yourself some of the following
questions:

1. What question is being asked of nature?

2. What measurements must be performed to answer this question?
3. What pitfalls exist? What variables are keep constant?
4. What hazards are involved?

You will be given detailed instructions as to what is to be done before lab. These should
be followed! The simplest method is to make a summary in your notebook. Aim for
telegraphic simplicity. Leave a lot of space in the notebook, at appropriate places, for
measurements.

Preparation does not take place in the notebook, but in your head! Our studies have
shown that students who prepare well go home about 20 percent earlier, on the
average.

To give you an idea of how such a summary is prepared, a section of the lab manual,
together with the resulting student summary, is now presented.

Preparing Your Notebook Before Coming to Lab

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This is in the original procedure, taken from the procedure for the synthesis of
Tetraiodomercurates.

1. You will be given a test tube containing 30 mg of Hg2+ in an acid medium. This
solution is poisonous.

2. To the solution in the original test tube, add 1 mL of 0.5 M KI solution. Agitate for 30
sec or so. A solid (HgI2) will form and then gradually dissolve to form Hgl42-. You
should not need more than about 1 mL. If the solid does not completely redissolve after
about 30 sec, add more KI solution drop-wise, agitating after each drop until a
transparent solution results.

3. To the resulting solution, add 3 mL of 0.1 M Ag+ or 0.1 M Cu2+ solution, depending
on whether you are trying to make the silver or copper salt. A precipitate will form.
Agitate gently, taking care not to spill.

4. Heat in the water bath to "digest" the precipitate for 5 to 10 min. During digestion,
small crystals dissolve and larger ones form. Let the solution cool and settle.

5. With a disposable dropper, remove most of the liquid, discarding the liquid into the
"mercury waste" container in the hood. Add 2 to 3 mL of distilled water and bring to
the boil. Again, cool, let the solid settle, and discard the waste solution into the mercury
waste container.

6. Add a few drops of distilled water. Use the tip of a disposable dropper to stir up the
precipitate and suck up the solid. Transfer it to a clean 50 mL beaker. Allow the beaker
to stand uncovered for a week in your desk. This will allow the excess H2O to
evaporate.

The following is an example of how the procedure appeared in a student's notebook.

o Receive test tube with 30 mg of Hg2+ (poisonous).

o Add 1 mL of 0.5 M KI sol. and shake 30 seconds.
o Solid should form, redissolve. If solid not completely redissolved, add more KI drop-wise
until solution is transparent.
o Add 1 mL of 0.1M Ag+ or 0.1 M Cu2+, agitate.
o Heat 5 to 10 min in H2O bath.

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 o Let solution cool, and solid settle. Remove liquid with disposable dropper, discard into
"Hg waste."
o Add 2 to 4 mL of H2O. Heat to boil in H2O bath.
o After solid settles, remove and discard H2O into "Hg waste.”
o Add few drops H2O, stir up solid with dropper, suck up drop into beaker, let stand one
week.
o Observe and record colors.

The previous is a good notebook summary because

1. it is broken up into individual steps and has a check-list quality;
2. all key landmarks are present (for example, "solid should form, redissolve") so that
the student can check the results as the work goes on;
3. hazards are included;
4. there is a reminder to record crucial observations.

This summary could be written on the left-hand half of the page, leaving the other half
page for observations. Alternatively, the student could entitle it “To Be Done” and then
record measurements and observations at the end under the heading “What Was
Done”.

WORKING SAFELY

We have done our best to build safety into the design of the experiments and work
areas, but working in the lab still has risks. Your instructor will undoubtedly bring
safety rules to your attention. The ones listed below, which are universal, serve as a
starting point.

1. Wear eye protection at all times. If you ponder for a moment what would happen to
the rest of your college and professional career if you were accidentally blinded this
very period, I am sure you will agree that the discomfort of safety glasses is a small
price to pay for some added insurance. In any case, you must wear eye protection
because it is mandated by federal regulations. If you refuse to wear eye protection, you
cannot come to lab. It is that simple.

2. Wear shoes that cover your feet (not open-toed or open-heeled shoes, or sandals).
This, too, is mandated by federal regulation. Do not wear shorts or skirts in the lab.
Wear long pants. Shoes and clothes provide a first line of defense against spills. Old

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blue jeans are a good choice for lab clothes. They resist chemicals, and stains on them
are not noticeable. If all else fails, they can be thrown out at the end of the semester.
You will also be required to wear a lab apron when working in the lab.

3. Do not eat, or drink, in the lab. As the alchemist Paracelsus remarked, "All things are
poisonous, for there is nothing without poisonous qualities. It is only the dose which
makes a thing poison." These words are as true now as in the sixteenth century. If you
need to eat, or drink, do it in the hall. Although few chemicals are absorbed through
your skin, avoid touching chemicals whenever possible. Wash your hands at the end of
the lab period.

4. Be aware that burns and fires are serious hazards. Some of the substances that you
work with burn very easily. Also note that hot glassware looks very much the same as
cold glassware, but its effect on your skin is very different!

5. Do not perform any unauthorized experiments. Ask permission first. The difference
between using potassium chlorate and chloride may be an explosion!

6. Report even trivial injuries to your teaching assistant or lab supervisor. What seems
minor can have major complications.

7. Work in the lab only if you are being supervised. You can work only during your
scheduled lab period, unless other arrangements are made, and even then, you may
work only in the presence of a teaching assistant.

8. Know the location of emergency exits, emergency showers, eye-wash fountains, and
fire extinguishers. Always know two different ways out of a lab. Do not put book bags
or other things on the floor, where they might impede escape. In a real emergency,
follow the instructions of teaching assistants or supervisors. Move, do not argue!

9. Do not, as a rule, bring visitors into the laboratory. Ask permission before bringing
them, and see that they obey the rules. You can always talk in the hall.

10. Do not listen to music through earphones. (You want to be able to hear instructions
in an emergency.)

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If you are, or might be, pregnant, consult your instructor about postponing your lab. All
chemicals known to cause birth defects at this writing have been excluded, but so little
is known about this topic that a conservative approach seems appropriate. The threat of
birth defects from toxic agents is most serious in the first 3 months; it seems that the
hazard is much less later.

When you notice a fellow student who is not following rules, remind him or her.
Almost certainly, your fellow student would rather be reminded by you than by a
teaching assistant or faculty member! If you are the one being reminded, thank the
person doing it and be glad you did not find out "by accident."

Using Proper Lab Etiquette

Lab work can be made faster, pleasanter, and simpler for everybody if your class can
use peer pressure to encourage people to observe some rules that fall into the category
of etiquette. For example, do not remove tools and reagents that are to be shared. Do
not stick droppers or other tools into stock solution bottles. If you spill something,
clean it up. At the end of the period, sponge off your bench, so that the next user does
not have to start by cleaning up a puddle of colorless liquid, wondering, "Is it water or
sulfuric acid?"

USING THE TOOLS OF THE TRADE

Bunsen burners, beakers and test tubes are a few of the tools you will use for the
following experiments.

Running a Reaction

To run a reaction, you will need to combine the chemicals (called reagents) and possibly
to mix them. These basic techniques are covered in this section.

How to Adjust a Bunsen Burner

In order to accurately perform an experiment using a Bunsen burner, the flame needs
the proper mixture of gas and air. The flame will be noisy or blow out if there is too
much air or not enough gas. A smoky or yellow flame indicates that there is too much

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gas or not enough air. Regulate the air by adjusting the barrel. Control the gas with a
needle valve in the burner base.

How to Set Up a Beaker or Flask for Boiling

Place a piece of wire gauze on a tripod, then place the beaker or flask on top of the wire
gauze. The gauze helps support the beaker and also spreads the heat. To stop the heat,
remove the lighted burner from under the flask, then let the contents of the container
stop boiling before attempting to pour or remove. Use beaker tongs or crucible tongs to
grasp a hot object.

Bumping

Boiling may be uneven and explosive. This phenomenon, known as bumping, is

controlled by adding boiling chips. These stones act as nuclei, giving the vapor bubbles
a place to form so that the liquid does not superheat. Before adding boiling chips,
always let the hot liquid cool below the boiling point. Otherwise a burst of boiling will
occur when the chips hit the liquid, often scattering the liquid out of the container.

How to Work with a Test Tube

Many of the experiments in this lab manual are done in test tubes. To mix solutions, or
to get a solid to dissolve, do not seal the test tube with your thumb and invert it. This
will contaminate the solution and may be dangerous to your skin. Rather, grasp the top
of the test tube firmly and then tap rapidly with a finger from the other hand. Use a
circular stroke, letting your finger quickly slide down the outside of the tube (Fig. 1). If
you do this correctly you can create a vortex in the test tube that will mix it efficiently.

Never heat a test tube directly. Always immerse it in a hot water bath. Otherwise the
liquid may bump and fly out of the test tube.

Figure 1 Mixing solutions in a test tube

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MEASURING MASS

Many of the measurements in this manual depend on the analytical balance, which is
potentially one of the most accurate instruments available to you. Learn to use this
balance well. Your teaching assistant will explain how to use the particular model of
balance available in the labs.

How to Use the Analytical Balance

Whenever you are asked to measure the mass of a solid, you will be given a range of
mass values. Any mass in this range will work, as long as you know exact mass of the
solid transferred.

Measuring Mass by difference. Put the solid in a vial, put the top on the vial (to keep
out moisture and dust), and take an initial reading, this is called the tare. Reset the tare
to zero, and transfer a small amount of the solid into a beaker or flask and reseal the
vial. Pour the solid directly into the beaker or flask; do not use a spatula lest some of
the solid stick to it. Remeasure the mass of the sealed vial. The negative reading on the
balance is the mass of the sample transferred. If the amount transferred is not sufficient,
transfer more to the beaker and remeasure the mass of the vial. If you have added too
much, clean out the beaker and start over. Do not transfer the solid back to the initial
vial lest you contaminate the entire sample. Alternately, you can record the initial and

9
final mass of the sample, and the difference between the two masses is the mass of the
sample transferred.

Remember that the analytical balance is a very precise instrument. Always record all of
the available decimal places. You can round off the number later.

For precise work, do not weigh hot objects on the balance. A hot object creates
convection currents of air that cause the reading to appear light. Although many books
suggest holding objects only with tissue, this is unnecessary unless you have very
sweaty fingers. Hugging the sample in the palm of your hand is not recommended and
will lead to a steady downward drift as the moisture evaporates.

The area in and around the balance must be kept clean. Spills are expected, and you
will never be penalized if you clean them up. However, leaving a mess for the next
student is discourteous and dangerous.

How to Use the Beam Balance

The beam balance is used for rough measurements only and should not be used unless
specified explicitly in this book. Directions vary from balance to balance, and your
instructor will advise you in using yours.

MEASURING VOLUME

Learning to do good volume measurements is essential, and not difficult.

How to Clean Glassware

Soap and water will remove almost all of the stains you will have on glassware (except
as noted for KMnO4) in this course, although it may take some scrubbing. Labels can be
removed by soaking in hot water and then scraping with a spatula, using the same
motion as that for peeling an apple.

It is not necessary to use a great excess of soap. Excessive amounts are difficult to
remove and require many rinsings, which takes time. Do the final rinsing with a small

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amount of distilled water (just enough to thoroughly wet the inside, but not enough to
fill or even halfway fill the container).

How to Take Solutions from Stock Bottles

Use a graduated cylinder to take solutions from stock bottles. Pour the stock solution
from the stock bottle into the graduated cylinder, until you have taken slightly more
than you need. Take the cylinder to your desk, and remove the excess with a dropper.
Never, never pour the excess back into the stock bottle. Never, never put any object (for
example, a dropper) into the bottle. If you encounter difficulty with a bottle, notify
your TA or instructor.

Remember this as the "one-way" rule: Things come out of stock bottles but never go
into them!

Do not take stock bottles to your desk. Also, if bottles have been placed in the hoods,
leave them there. The hood helps confine poisonous, smelly, or corrosive spills.

How to Use a Volumetric Flask

A volumetric flask must never be heated, because it will probably break. Even if it does
not break, the volume calibration will be destroyed. Dissolve solids before adding them
to the flask, rinse container used for the solutions with a wash bottle, and add the
rinsings to the flask. Swirl the flask to thoroughly mix the solution after each addition
of rinsings. For good control, add the final drops of the liquid with a pipet, not a squirt
bottle. After filling up to the mark (a circular ring etched on the neck), insert the
stopper, and invert the flask to thoroughly mix the solution. You cannot mix too much,
but each year many students have difficulties because they did not mix enough! If you
fill the flask past the mark, discard the solution and start over (Fig. 2).

Do not store solutions in volumetric flasks. The solution may cause the stopper to
"freeze,” that is, to become solidly wedged in the flask. If this happens, get assistance
for frozen stoppers.

Figure 2 A Volumetric Flask

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An Interpretation of the Hieroglyphics on a Volumetric Flask

A
TC 250 mL ± 0.12 mL
20 °C
Pyrex® USA No. 5640

A volumetric flask is calibrated to contain a certain volume of solution at 20 °C when

diluted to mark. The inscription above appears on a typical volumetric flask. What
does it mean? The top line, A, means “Class A” according to the National Bureau of
Standards. The next line means “To Contain at 20 °C, 250 mL with an absolute
uncertainty of ±0.12 mL.” The third line means “made of Pyrex glass (a registered
trademark for a type of borosilicate glass) made in the United States, Catalog No. 5640.”
Note that the old abbreviation ml is now being replaced by mL.

Accurately Measuring Volume with a Buret.

Beads of water form on the inside of an unclean buret when it is wet, as a result of an
invisible layer of grease. This may interfere with the accuracy of the measurement,
because drops remaining on the side of the buret will be counted as if they had been
delivered.

After rinsing the buret, including the top, several times with water, rinse it with a little
of the solution you will use. This prevents accidentally diluting the solution. Fill the
buret over your sink, which you should be able to do without a funnel and without

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spilling. (Funnels can introduce contamination, unless they, too, are rinsed with a little
of the solution to be transferred.) Run some of the liquid until the tip of the buret is
filled and the meniscus is on scale. It is a waste of time to start at 0.00 mL.

To read the buret, look at the bottom of the liquid meniscus and then “guestimate” the
last place, so that you have a reading with two places after the decimal. The volume
delivered is the difference between the first reading and the final reading, and is
measured in milliliters (mL). The numbers increase reading down the buret, rather than
up as on a thermometer (Fig. 3).

If you cannot remove all the air from the tip, you may get a false reading when it fills up
later. To remove an air bubble, hold the buret over the sink, open the valve, and shake
once vertically. Ask the teaching assistant for help if you are having trouble.

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 Figure 3 Buret Reading

Pipeting

Two sorts of pipettes are available: the measuring pipette, which is often used in clinical
medicine and has graduations along the side, and the transfer pipette, which has a
bulge in the center. The latter is much more accurate. To use a transfer pipette, follow
this procedure.

1. Clean it thoroughly to prevent beads of water from clinging to the inside. These
beads count as delivered, even though they remain inside.
2. Hold the pipet with one hand and the pipet bulb with the other, squeeze out the air
from the bulb, then loosely attach it to the top of the pipet until the liquid has been
pulled up above the mark. Quickly remove the bulb and put your finger over the top of
the pipette.
3. Gently rock your finger back and forth without lifting it off the top of the pipette so
that you slowly let the liquid level fall until the bottom of the meniscus just touches the
line. Release the top of the pipette, and let it deliver the solution into the vessel. Touch
the tip to the side of the container, and hold it there for a few seconds after it looks as if
all the contents have drained out. Do not blow out the pipette or put your mouth on it
at any time.

What Do “To Contain" and “To Deliver" Mean?

Volumetric flasks are, of course, calibrated to contain the stated volume. Transfer
pipettes, those with no graduations on the side, are calibrated to deliver and are marked

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“TD”. Other pipettes are usually marked to contain. Transfer pipettes need not be
blown out.
DISPOSING OF WASTE

There is a patchwork of state, federal, and local laws about waste disposal, and this is
constantly changing. Your instructor will inform you of the proper method for
disposing of chemical waste. Please comply with these rules-they make the world safer
for all of us.

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Experiment 1: Co-crystallization of an Organic dye with
Kalinite.

A crystalline solid is composed of an identical pattern of atoms, ions and/or molecules.

Usually the crystallization process is selective and atoms, ions or molecules of the
wrong shape or size or charge will not be incorporated into the crystal lattice.
However, a different molecules or ion of the correct size and charge can be incorporated
into the growing crystal through a process called co-crystallization.

Kalinite, KAl(SO4)2•12 H2O, is a colorless solid that is easily synthesized from Al metal.
Since Kalinite readily forms crystals, it is ideal for this experiment. In this experiment
you will synthesize, and purify Kalinite, and then determine which (if any) of two
organic dyes, Bismark Brown and Bromo - Cresol Green, cocrystallize with Kalinite.
Since the dyes are colored, while Kalinite is colorless, it is easy to determine if
cocrystallization occurs.

Chemistry of Kalinite Synthesis:

The synthesis of Kalinite starting from Al metal is outlined in the four equations below.
N.B. These reactions are not balanced. You need to balance these reactions for the lab
report.

Al (s) + KOH (aq) ⟶ KAl(OH)4 (aq) + H2 (g) (eqn 1)

KAl(OH)4 (aq) + H2SO4 (aq) ⟶ Al(OH)3 (s) + K2SO4 (aq) (eqn 2)

Al(OH)3 (s) + H2SO4 (aq) + K2SO4 (aq) ⟶ Al2(SO4)3 (aq) + K2SO4 (aq) (eqn 3)

Al2(SO4)3 (aq) + K2SO4 (aq) ⟶ KAl(SO4)2 • 12 H2O (s) (eqn 4)

The rapid dissolution of aluminum metal in a warm aqueous solution of potassium

hydroxide (KOH) produces hydrogen gas, and the aluminate ion (Al(OH)4-) in an
exothermic reaction, (eqn 1). Aluminum is an example of an amphoteric metal. It is
soluble in both an acidic and basic solution. Most metals, iron for example, are only
soluble in acidic solution and form precipitates in basic solutions. In equation 1 the

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aluminate ion, Al(OH)4- , is the soluble form of aluminum in basic solutions. Since the
desired product is in solution, any insoluble impurities can be filtered away at this step.

Treatment of the filtered solution with sulfuric acid first produces a gelatinous
precipitate of aluminum hydroxide (Al(OH)3) (eqn 2), which then dissolves as more acid
is added (eqn 3).

The kalinite is not very soluble in methanol, so the addition of the solvent will induce
precipitation of the desired material from solution. Isolation of the solid and
purification by recrystallization from water will yield pure Kalinite. (eqn 4).

Preparation of Kalinite:

CAUTION: Potassium Hydroxide, KOH, and Sulfuric Acid, H2SO4, are corrosive and
must not be allowed to touch the skin, eyes or clothes. Methanol, CH 3OH, and
Ethanol, C2H5OH, burns easily; keep fire and flames away when working with them.

1. Accurately weigh between 0.2000 - 0.2500 g of alloy chips and transfer to a medium
sized test tube. Add 10 mL of 1.4 M KOH solution (be careful not to get any KOH
solution on your skin. If you do, immediately wash with water), and warm the solution
in a warm water bath. Be careful not to BOIL this solution. After 20 - 30 min remove
the test tube from the water bath and allow the test tube to cool. Remember to record
all observations (i.e. color changes, evolution of gases).

2. Gravity filter the cooled solution into a small beaker. To the filtrate carefully add 5
mL of 9 M H2SO4 (be careful not to get any H2SO4 solution on your skin. If you do,
immediately wash with water). If a precipitate still remains after all the acid has been
added, warm the solution again, until all the solid is dissolved.

3. Get 10 mL of methanol from the hood. Before bringing the methanol back to your
bench, make sure there are no flames in the immediate vicinity. Methanol Burns! Place
the beaker in an ice bath, add the 10 mL of methanol to the solution, and allow the
solution to cool for 10 - 20 min. During this time crystals will form. Collect the crystals
by vacuum filtration using a Buchner funnel. Your TA will demonstrate how to
perform a vacuum filtration.

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Purification of the Kalinite:

The crude kalinite contains a small excess of K2SO4 impurities, and these crystals will be
purified via recrystallization from water. Recrystallization is the most common method
for purifying a solid material. This method takes advantage of the differences in
solubility of a compound in hot and cold solvent. The impure solid is dissolved in the
minimal amount of hot solvent and as the solution cools the pure product crystallizes
from solution leaving the impurities behind in solution.

Heat about 10 mL of distilled water. Place your Kalinite in a small 50 mL beaker, and
add the hot water drop wise with a disposable pipet until all the solid dissolves. It may
be necessary to warm the solution of water and Kalinite if it becomes too cool. When all
the solid is in solution, remove from the heat and allow the solution too cool. You can
place the beaker in an ice bath to speed the cooling process, but if you allow the solution
to cool slowly you will get larger crystals. Collect the solid on a Buchner funnel.
Obtain an exact weight of the dry crystals.

Cocrystallization with Organic Dyes:

Dissolve 0.10 g of purified KAl(SO4)2•12 H2O in a few mL of water in a small test tube.
(At this step it is OK to add an excess of water to dissolve all the solid.) Divide the
solution into three portions, placing the portions on three separate, labeled watch
glasses. Add 2 - 4 drops of dye solutions to two of the watch glasses, keeping the third
as a control. Allow the watch glasses to stand for a week in your locker. The following
week wash the crystals with methanol in the hood. Note any color changes in the
crystals.

For the Lab Report

1. Write balanced equations for the formation of KAl(OH)4 (eqn. 1), Al(OH)3 (eqn. 2),
Al2(SO4)3 (eqn. 3), and KAl(SO4)2•12 H2O (eqn. 4).

2. The percent yield is a measure of the efficiency of a chemical reaction, and is defined
below. The actual yield is the number of grams of dry crystals of Kalinite you recorded.

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 actual yield
% yield= × 100
theoretical yield
The theoretical yield is the number of grams of product that would be obtained if the
reaction went to 100% completion and produced only the desired product. The
theoretical yield for this reaction can be determined as follows:

a. Since the aluminum is the limiting reagent, calculate the number of moles of
aluminum that you started with. The alloy chips used in this experiment are 92 %
pure aluminum.

b. Since the mole ratio of Al : Kalinite is 1:1, calculate the number of grams of
Kalinite produced if the reaction went to 100% completion. Molecular weight for
Kalinite is 474.39 g/mol

mass alloy chips 1 mole KAl(SO4 )2 •12 H2 O 474.39 g

theoretical yield = 0.92 ( )( )( )
atomic mass Al 1 mole Al mole

From the above formula and your data, calculate the percent yield for this reaction.
Explain briefly whether the yield that you calculated is feasible.

3. The ion Fe3+ is very similar in size to Al3+ and can replace it in the crystal lattice of
kalinite, so that kalinite with an iron impurity is common. Explicitly describe how can
one produce pure kalinite from contaminated kalinite? (Hint: first dissolve the kalinite
in water then add something that will precipitate the iron.)

4. Which organic dye co-crystallized with the kalinite? Explain your reasoning using
your observations.

19
Experiment 2: Preparation of a Standard Sodium Hydroxide
Solution

This experiment describes the preparation and the standardization of a Sodium

Hydroxide (NaOH) solution, and the titration of an unknown acid to check the accuracy
of the NaOH solution.

Why not just dissolve a measured mass of NaOH in a Volumetric flask?

Sodium hydroxide has the awkward property of absorbing moisture and CO 2 from the
atmosphere. It is impossible to make a solution of an exact molarity by weighing the
sodium hydroxide alone because the sodium hydroxide pellets contain an unknown
quantity of impurities.

The easy way to solve this problem is to titrate the NaOH solution against a primary
standard. A good primary standard should be a high molecular weight solid that is
easy to handle and weigh. Also, the primary standard should not pick up moisture
from the air. In this experiment, potassium hydrogen phthalate (pronounced “thallate”,
and abbreviated KHP) will be used as the primary standard.

Chemistry:

The reaction of NaOH with KHP is shown below. The balanced equation shows there is

H H

H C COOH H C COONa
C C C C
+ NaOH + H2O
C C C C
H C COOK H C COOK

H H
potassium hydrogen
phthalate (KHP)

a 1:1 stoichiometric relationship between NaOH and KHP. The molarity of the NaOH
solution can be calculated from the recorded volume of NaOH solution required to

20
neutralize a known mass of KHP. This method of determining accurate concentration is
called Standardization.

The procedure requires knowing exactly when the neutralization reaction has occurred.
This problem is solved by using an indicator, a dye that will undergo a rapid, reversible
molecular rearrangement in solution. There is a conspicuous color difference between
the molecular forms in acidic and in basic solutions, and the colors are so bright that
only a little of the indicator need be used. A single drop of NaOH solution will convert
some of the dye from its acidic form to its basic form so the first excess of NaOH not
used to neutralize the acid will convert the dye to its basic form, which is brightly
colored. This result indicates that neutralization reaction has occurred. This point is
known as the end point of the titration.

How to measure volume accurately.

This experiment hinges on the accurate measurement of volume, which can be done
most easily by using a buret. Learn to use this tool efficiently and accurately.

Beads of water will form on the inside of an unclean buret when it is wet, because of an
invisible layer of grease. This interferes with the accuracy of the measurement, since
drops remaining on the side of the buret will be counted as though they had been
delivered.

After you have rinsed the buret (including the top) several times with deionized water,
rinse with a little of the solution you will use. This prevents the accidental dilution of
the solution you are adding. Fill the buret over the sink. You should be able to do this
without a funnel and without spilling. (If you must use a funnel, rinse it with a little of
the solution to be transferred.) Run the liquid until the tip of the buret is filled and the
meniscus is on scale. If an air bubble persists in the tip, open the valve and shake the
buret once vertically with a snap of the wrist. There is no need to start at exactly
0.00 mL.

To read the buret, look at the bottom of the liquid meniscus and then “guestimate” the
last place, so that you have a reading with two places after the decimal. The volume
delivered is the difference between the first reading and the final reading and is
measured in milliliters (mL). Note that the numbers increase as you read down the

21
buret, not up as on a thermometer. See pages 12 and 13 to review instructions for
accurately reading a buret.

Last, be sure, when filling, to write down the concentration and any other information
appearing on the stock bottle label.

22
Part A: How to prepare the NaOH solution.

CAUTION: Sodium Hydroxide, NaOH, is corrosive and must not be allowed to touch
the skin, eyes or clothes. Clean up any spills, and rinse skin with water. Inform your
TA of any spills.

A stock solution of concentrated NaOH will be provided. Keep this material off your
skin and clothes, and promptly clean up spills! Add about 30 mL of this solution to 900
mL of distilled water in a clean plastic bottle, stopper and mix well.

Mixing well means shaking the bottle for at least 1 full minute with as much vigor as
you can muster – more shaking does no harm. The diluted NaOH, while poisonous, is
not nearly as corrosive as the concentrated solution.

Part B: Standardizing the NaOH solution with KHP.

Take the plastic vial containing your KHP to the balance with a conical flask. Measure
the mass of the vial to record the exact mass. Tare the balance, and transfer between
0.5000 g and 0.8000 g of solid to the flask, and in your notebook, record the exact
amount transferred to the flask. Do not use a “scoopula” to transfer the solid from the
vial to the flask. Pour the solid directly into the flask. Add about 50 to 100 mL of
deionized water to the conical flask. Warm to dissolve, and add 3-5 drops of
phenolphthalein indicator.

Fill a buret with the diluted NaOH you prepared, ensuring to check for no air bubbles
in the tip, then record the initial reading. Now add NaOH solution from the buret to
the flask, quickly at first while swirling. It is useful to swirl with your dominant hand
and control the volume on the buret with your nondominant hand. Continue adding
the solution drop-wise as you approach the end point. The pink color of the indicator
will persist for an increasingly longer time, and will finally spread through the solution.
Record the final volume of NaOH solution added to reach the pale pink end point.

Repeat this procedure until you have measured two satisfactory end points. The
following runs will proceed quickly after the first run. Compute the exact NaOH
concentration (see next section), and label your bottle. Keep the NaOH in your desk. You
will need it for subsequent work.

23
Calculating the Concentration of Sodium Hydroxide

The calculation depends on the important fact that one mole of KHP will neutralize
exactly one mole of NaOH. Then at the endpoint, the moles NaOH will equal the moles
of KHP.

1. The molecular weight of KHP is 204.22 g/mol. Compute the number of moles of
KHP weighed out.

The concentration of NaOH is simply the number of moles of KHP per the number of
liters of NaOH solution run out of the buret.

The concentration or Molarity (M) of the NaOH solution can be calculated, and the unit
for Molarity is mol/liter:

mass KHP 1
Molarity NaOH= ( )
204.22 g/mol vol. NaOH

The volume must be expressed as liters (1 mL is 0.001 L) if the units are to work out.

2. Do the uncertainty calculations. Start by calculating the upper and lower limits for
your best run. If uncertain as to which is best, choose the last one because practice may
cause an improvement. For KHP samples weighed by difference, the uncertainties in
weight of KHP will be ± 0.0010 g. The two worst cases for the Molarity of the NaOH
solution will be

upper-limit mass KHP 1

upper-limit Molarity NaOH= ( )
204.22 g/mol lower-limit vol. NaOH

lower-limit mass KHP 1

lower-limit Molarity NaOH= ( )
204.22 g/mol upper-limit vol. NaOH

You should be able to explain why these formulas work. (See the Mathematical
Operations section at the end of this manual.)

24
3. Are the two concentrations identical within uncertainty? If not, shake the NaOH,
refill the buret, and do a third run to see if you can obtain agreement. (The shaking is
recommended only because incomplete mixing is the most common student error.)
4. To determine if two titrations experiments agree within uncertainty, look at the range
of concentrations. One titration of NaOH should fit inside the range of uncertainty just
calculated. For example, if your range is 0.0876M to 0.0888M and your first value is
0.0879M, you have agreement. If not, at most one run can be correct.

Again, do not average two runs that do not overlap.

Part C: Proof of Method test of your NaOH Solution

The purpose of this experiment is (1) to provide you with a yardstick by which to
measure your titration technique before you embark on the titration of real unknowns,
and (2) to give you an idea of what the lab practical exam will be like.

You will be given a sample of an unknown acid and are to report the apparent
molecular weight. Remember to record the Unknown Acid Number written on the vial
label in your notebook.

Weigh a sample of 0.5000 g to 1.5000 g of unknown acid into a conical flask, recording
the exact weight. Add 50 – 100 mL de-ionized H2O to the conical flask, and swirl to
dissolve the solid. Add 3-5 drops of phenolphthalein indicator.

You handle the unknown acid in the same way you handled the KHP. The first run will
probably be overshot, but weigh out another sample. Initially you can go quickly until
you’re close, then drop-wise.

Calculating the Molecular Weight of the Unknown Acid.

The Unknown Acid has one replaceable hydrogen, and at the endpoint the moles of
NaOH will equal the moles of Unknown Acid. The molecular weight is the number of
grams per mole. Since we know the number of grams of Unknown Acid we started
with, and we measured the volume of NaOH solution to reach the pink endpoint, we
can calculate the molecular weight of the Unknown Acid by:

25
 mass Unknown Acid
Molar Mass Unknown Acid=
Molarity NaOH (vol. NaOH)

There is no uncertainty analysis required for the Unknown Acid titration. Your TA will
tell you where to check your value of the Unknown Acid molecular weight. If your
value agrees, then you have accurately determined the molecular weight. If your value
does not agree, then perform another titration.

For the Report

Set up a worksheet in Excel with the entries shown below. Fill in your data in the
appropriate cell locations. For example, the net mass of KHP you used in run 1 should
be entered in cell B3. Use as many or as few columns as necessary to include data from
all titration runs that you performed, even the ones with blunders.

Figure 2.1 Excel worksheet example for reporting NaOH titration data.

26
1. In Table 1, calculate the concentration of the NaOH solution for each titration and
perform an uncertainty analysis for each run using Excel formulas. Remember that the
uncertainty for a net mass is ± 0.0010 g and the uncertainty for a net burette volume is
± 0.10 mL. Check that your calculations are correct; they should match what you
calculated manually during your lab period.

2. Check that you have agreement between two runs in Table 1, that is the
concentration of NaOH value from one run falls between the lower and upper limits of
another run. Indicate with an “X” which runs agree in Row 10. The final concentration
you should report in Cell B12 is the average of the two runs that agree.

27
3. Report the uncertainty limits for the average final concentration you calculated.
Average the upper limits of the two runs to obtain the upper limit of the average.
Likewise average the lower limits to obtain the lower limit of the average. Again, do not
average two runs that do not agree.

4. For Table 2, calculate and report the molar mass for your Unknown Acid using Excel
formulas. You do not need to perform an uncertainty analysis for this part. Remember
to include your Unknown number of the acid by replacing “AXXX” in the table title and
headings.

5. When you have finished your calculations in Excel, copy and paste the Tables into the
Results section of your lab report. Also, use the Ctrl +` command you learnt in the Excel
lab to display your formulas. Make sure that the formulas are completely visible and
take a screen shot including the column and row headers (i.e. A, B, C, D, etc. and 1, 2, 3,
4, etc.). Paste this screen shot into the Calculations section of your lab report. Comment
briefly on the accuracy or precision of your data.

SAVE THE NaOH SOLUTION! YOU WILL NEED IT FOR

FUTURE WORK.

28
Experiment 3: Formula of a Mineral.

You are a nineteenth-century chemist. A geologist has just returned from a far-away
placed called California. Among the collection of mineral samples is one believed to be
novel. Preliminary tests confirm that the mineral is a sulfate. It probably contains
water of crystallization, but what metal does it contain? What is the formula of the
mineral? Perhaps it contains a hitherto unknown element (which you will have the
honor of naming).

The mineral has the following components: (1) a metal ion or ions, which is positively
charged, (2) the sulfate ion, which is negatively charged, and (3) the water of
crystallization. Over the next three lab periods, you will analyze your mineral to
determine the number of grams of each of these components in the sample. From this,
the formula of the unknown mineral and the atomic mass of the metal ion(s) can be
deduced.

Some of the minerals used in this experiment have an unfortunate property, that is, the
tendency to lose or gain water if exposed to the atmosphere for a prolonged period.
Keep the mineral sample in a sealed container. Only open it for only the minimum
necessary amount of time.

The analysis of the sample will take three 3-hr periods. It is recommended that you do
the calculations for each section as you complete it, so that if something looks odd, you
can consult your teaching assistant. Note that all of the measurements should contain
at least four significant figures; rounding off can yield strange results.

This seems to be a challenging experiment, primarily because for many students it

requires a precise chemical analysis. Plenty of time is allowed, you can repeat a step if
necessary. The reward at the end is the intellectual satisfaction of being able to identify
confidently the composition of this white powder.

Part A: Flame Test, a Quick Preliminary Test

Take a clean nichrome wire, make a loop and heat a single crystal of the mineral in a
flame. Your teaching assistant will demonstrate this operation. For comparison, heat
samples of NaCl and KCl to observe a positive test for Na+ and K+ ions. Ensure the wire

29
is cleaned in the flame before each test. If your mineral gives a bright color to the flame,
it may be possible to decide whether
1. It has sodium.
2. It has potassium.
3. It has an unknown element (another color flame or no color at all).
Note that if the flame test is positive for sodium, potassium may or may not also be
present. The sodium flame obscures the potassium color. This test takes only 5 or 10
min and can provide useful information.

Part B: Analysis for Water of Crystallization

A certain number of water molecules are needed to hold together the mineral crystal.
They are weakly bonded to the ions, and heating or sometimes simply exposure to a
dry atmosphere causes them to be lost. Usually the water of hydration has a definite
stoichiometric ratio to the ions in the salt. This loose bond between the water and the
rest of the ions is signified by the dot as, for example, in CaSO4 • 2 H2O. This is the
formula for gypsum and states that the crystal contains two water molecules for each
Ca2+ or SO42- ion. Often the color and hardness of the hydrated form of the crystal and
the anhydrous (water-free) form are strikingly different. A practical use for the
hydration phenomenon is the setting of plaster of Paris CaSO4 • ½ H2O. When mixed
with water, it slowly turns into solid gypsum.

How to Measure the Water of Hydration

You will do the reverse of the reaction just described in the plaster of Paris example.
You will take a hydrate and heat it until it is anhydrous.

The heating will be done in a crucible (not a filter crucible) which must always be
handled with crucible tongs, not with your hands or even with gloves. Any cooling
steps will be done in your dessicator. This is a device to keep objects free from
atmospheric moisture, and depends on a chemical drying agent, CaCl2. Check your
dessicator. Is the CaCl2 drying agent caked or moist? If so, it should be replaced. If the
seal is not tight, a little grease from the prep room will help.

30
1. Heat a small crucible and its cover for about 2 min on a clay triangle to dry it
thoroughly. Cool the crucible in your dessicator. When it is cool, determine the precise
weight of the crucible and cover.

2. Record your sample unknown number; these tend to smear so you should record this
number immediately upon obtaining the sample. After measuring the initial mass of
the vial, transfer between 0.5000 and 2.0000g of mineral to the crucible, and reweigh the
vial to find the exact mass transferred. Record the mass of the crucible and mineral as a
single measurement.

3. Place the crucible on the clay triangle, and put on the cover, so that it does not
completely cover the crucible but sits jauntily like a beret. Heat gently at first, and keep
the flame moving to avoid hot spots. Increase the heat moderately but do not permit the
crucible to become red hot. Overheating may cause the salt to decompose. Using crucible
tongs, occasionally remove the cover to see if the dehydration appears to be complete.
Observe any change in the appearance of the powder caused by the loss of the water
molecules. When the dehydration is complete (~15 min), continue to heat for another
five min.

3. Allow the crucible and contents to cool in the desiccator to prevent stray moisture
from being picked up. Weigh the sample accurately when cool; then reheat for 10 min
and see if a further decrease in mass occurs.

4. Repeat until the mass is the same, within uncertainty limits. Then you may be certain
that all the moisture has been driven off. This procedure is called drying to constant
mass. Remember that objects seem lighter when they are hot because of air currents
near the balance pan. Be sure to wipe off any stray drying agent clinging to the outside
of the crucible before weighing.

Strictly speaking, we have not shown that the only chemical change is loss of water.
This might be hard to prove. One could condense the water vapor and show that the
weight of water is equal to the loss of sample weight. Or, one could show that if water
is added to the anhydrous salt, the product is chemically identical to the original
mineral.

31
How to Do the Calculations for This Part

Make a table in your lab notebook showing the net mass of “wet” mineral you started
with and net mass of dry mineral you collected at the end of the analysis. Calculate the
net mass loss. Assuming the mass loss is only due to dehydration, you can calculate the
grams of H2O per gram of mineral (Gwater), and the moles of water per gram of mineral
(Mwater). These values are calculated by

mass water moles water Gwater

Gwater = Mwater = =
mass sample mass sample 18.015 g/mol

where the mass water is the mass lost by the mineral sample, and the mass sample is
the net mass of the wet mineral sample at the start of the analysis. The value for the
molar mass of water is 18.015 g/mol.

You will also need to show the upper and lower limits, and compute the range in the
final number Gwater and Mwater. Only the net mass of water lost and wet mineral sample
have uncertainties associated with them. See the section “Reporting your results” to
get started on your Excel calculations for this part of the experiment.

Part C: Sulfate Analysis

We need to know how many grams of sulfate ions are in each gram of mineral. Clearly,
it is not possible to separate the SO42– ion and measure the mass of sulfate.

In this situation, chemists use a technique called gravimetric analysis. One forms an
insoluble compound with the ion in question and collects the precipitate from the
solution. Your analysis will exploit the fact that BaSO4 precipitates out until virtually
all the sulfate ion has been removed from the solution. Then it is a simple matter to
filter out the solid BaSO4 and weigh it. The number of moles of BaSO4 formed will
equal the number of moles of SO4 2- present. The balanced equation is shown below.

32
Note that the BaCl2 totally dissociates to the Ba2+ and Cl– ions, and no harm is done if an
excess of Ba2+ ions are added to the solution.
A gravimetric analysis can be made very accurate because the analytical balance is
potentially one of the most accurate instruments we have available. An accurate mass
of BaSO4 is all that is needed to accurately calculate the number of moles of sulfate in
the original mineral sample.

How to Do the Sulfate Analysis

CAUTION: Concentrated Hydrochloric Acid, HCl, is corrosive and must not be

allowed to touch the skin, eyes or clothes. Clean up any spills, and rinse skin with
water. Inform your TA of any spills.

1. Measure the mass of the original sealed vial containing your mineral sample.
Transfer about 0.2000 to 0.5000 g to a clean but not necessarily dry 250 mL beaker.
Reseal the vial and measure the mass of sample transferred. (If you go modestly over
0.7 g, you can still save the experiment by adding proportionately extra BaCl2 . More
than 0.7 g will yield so much product that filtering will be very slow. Clean out the
beaker and begin again.) If your sulfate mineral is only marginally soluble in water,
you may find that even 0.2 g is too much and that you need much smaller samples.

2. To the beaker add 100 mL of deionized water and 3 - 5 drops of concentrated HCl.
Bring to the boiling point, then remove the burner so that the liquid stops boiling.
Obtain 10 mL of BaCl2 solution in your graduated cylinder. Once all of your compound
has dissolved, add a drop of 0.5 M BaCl2 solution, and swirl. Then add the remaining
10 mL of BaCl2 solution. This method creates larger and more easily filterable crystals
of BaSO4. Cover the beaker with a watch glass and boil gently for at least 5 min. Then
let the beaker stand for a few minutes. The boiling process enables the small crystals of
BaSO4 to dissolve and larger ones to form, a process called digestion.

3. While you are waiting for the digestion process to take place, examine a filter
crucible. Check to see if they have cracks in the fritted bottom by holding them up to
the light. If it is necessary to clean them, put them in the oven to dry for 1 hr afterward.
Do not weigh with a wet frit! Measure the mass of a clean, dry filter crucible. When the
digestion process is completed, filter the suspensions of BaSO4 through the crucible.
Your teaching assistant will demonstrate the best method. Speed up the filtration by
allowing the solid to settle completely and pouring the supernatant liquid through the
filter first.

33
Use a rubber policeman to scrub the inside of the beaker, and use the jet of water from a
wash bottle to direct the solid into the crucible (see figure 3.1 below). You must transfer
ALL of the solid to the filter crucible, and if any is spilled, discard the sample. Run
about 5 mL of water through the filter crucible to "wash" the sample, that is, to remove
any ions clinging to the solid. Your teaching assistant will show you how to use the
vacuum line to dry the solid in the crucible. Put your crucible in a 100 mL beaker, and
give your teaching assistant the beaker with a label inside that has your name on it. Use
a regular pen, not an eraseable pen, to write your name on the label. The sample will be
oven dried to eliminate the last traces of water. After the crucible has cooled, you will
measure the mass of the crucible and sample in order to determine the weight of BaSO4 .

Figure 3.1 Final Transfer of BaSO4 to Filter Crucible

One can do a gravimetric analysis only when no interfering ions are present. In this
precipitation, acid (HCl) is added to destroy any carbonate ion (by converting it to
carbon dioxide (CO2), which will bubble off) and any hydroxide ion (by converting it to
water). Both barium hydroxide (Ba(OH)2) and barium carbonate (BaCO3) are insoluble
in water and would have been collected on the filter with the BaSO4 desired. Thus,
hydroxide and carbonate are "interfering" ions for this analysis. The interfering ions are

34
different for each type of precipitation. Systematic errors result whenever the reagent
precipitating the ion you wish to measure precipitates stray ions as well.
How to Do the Calculations for this Part

The calculation relies on the known relationship between the mass of BaSO4 and the
amount of sulfate in the sample. From the balanced equation, we see that the BaSO 4
and SO42- have a stoichiometric ratio of 1:1. See the section “Reporting your results” to
get started on your Excel calculations for this part of the experiment.

1. Convert the net mass of BaSO4 to the number of moles of BaSO4 by using its molar
mass (233.4 g/mol). The number of moles of SO42- in BaSO4 is equal to the number of
moles of BaSO4. Therefore, the number of grams of SO42- is the number of moles
multiplied by its molar mass, 96.06 g/mol. This is also the number of grams of SO42- in
the original mineral sample. Divide the mass of SO42- by the mass of sample used in this
part of the analysis to get the fraction of sulfate, G sulfate.

mass BaSO4 96.06 g/mol

Gsulfate = ( )( )
mass sample 233.4 g/mol

2. Calculate the moles of sulfate per gram of mineral Msulfate by dividing Gsulfate by the
molar weight of SO42-.

moles sulfate Gsulfate

Msulfate = =
mass sample 96.06 g/mol

3. Calculate the upper and lower limits for the values of Gsulfate and Msulfate. Only the net
mass of BaSO4 and mineral sample have uncertainties associated with them.

Part D: Analysis of Metal Ion

This section of the experiment requires a NaOH solution of a precisely known

concentration. You will use your solution prepared in the Preparation of a Standard
Sodium Hydroxide Solution experiment. Complete that experiment first!

The Problem in Brief

35
You need to know how much of the mineral is metal ion. This isn't easy because all the
elements are different. If you don't know what the element is, how can you choose a
method - one that would work for any of them?

The answer is ion exchange. Instead of analyzing the metal ion directly, we will
"exchange" the metal ions for H+ ions, which we do know how to analyze. An ion
exchange resin has the remarkable property of exchanging any ion for a H+ on a charge
equivalent basis.

How "Ion Exchange" Works

Ion exchange is a process in which ions of the same type of charge (positive or negative)
are traded (exchanged) between a solution and an insoluble solid. Clays are among the
common solids that show this property, which is important for the retention of plant
nutrients like potassium. Chemists have improved on nature by creating ion-exchange
"plastics" or resins; these resins are porous and" have a large" capacity for holding ions.

There are two types of resins. Cation exchange resins are materials that contain many -
SO3H or -COOH groups that can exchange the cation H+ for other positive ions. Anion
exchange resins have groups such as -N(CH)3+OH- or -N(CH3)+Cl- that exchange OH- or
Cl- anions for other negative ions. Each location where exchange can occur is called an
exchange site. One long chain molecule may have many exchange sites.

When one ion is exchanged for another, electrical neutrality must be preserved. Ion
exchange resins work by substituting one type of cation (anion) for an electrically
equivalent quantity of another cation (anion). For example, if a table salt (NaCl)
solution is passed through a cation exchange column, HCl emerges from the column
since the Na+ ions are replaced by H+ ions. Conversely, NaOH emerges if NaCl is
passed through an anion exchange column because OH– ions replace the Cl– anions.
(Water is "deionized" by passing it first through a cation exchange column and then
through an anion exchange column. The first converts NaCl to HCl and the second
changes HCl into HOH, water.)

Since the reaction of ion exchange is reversible, it is possible to "recharge" an exchange

column that has exhausted its supply of exchange ions by treating the resin with a more
concentrated solution of H+ (or OH-) ions in the reverse process. These cations are
exchanged for Na+ (or Cl-) ions on the column.

36
 Figure 3.2 Ion Exchange Column

SO3 H SO3 H
+ M2+ + H+
SO3 H SO3 M+

before exchange after exchange

Ion exchange columns are used

1. To produce ultrapure deionized water for laboratory use and to desalt sea water.
2. To convert the salt of an acid (base) into the corresponding acid (base). The
concentration of the original salt solution can then be accurately determined by
titrating the acid (base).
3. To convert one salt into another, for example, to exchange K+ for Na+, a process often
important in making pharmaceuticals.

How to Run the Ion exchange on the Mineral

CAUTION: Sodium Hydroxide, NaOH, and Hydrochloric Acid, HCl, are corrosive
and must not be allowed to touch the skin, eyes or clothes. Clean up any spills, and
rinse skin with water. Inform your TA of any spills.

You will be loaned an ion-exchange column containing resin. Throughout this

experiment the column must not be allowed to run dry, because this creates channels
through which solution can run without being exposed to the resin. Run all substances
through the column slowly. (How slow is slow? You should be able to count the drops.)

37
The ion-exchange column should be filled with H+, although it is best to convert it again
to ensure that all the sites are protonated. Check to see that there are no air bubbles in
the resin before beginning. Drain the liquid until it is within ~1 inch of the top of the
column. Add a total of about 100 mL of 3M HCl to the column, allowing it to drain
slowly, topping up to keep the liquid level ~1 inch above the resin. Next wash the resin
with at least 100 mL of deionized water using the same process. After the rinsing, collect
a drop of the water emerging from the column (the eluate) in a clean watch glass. This
drop should become only faintly cloudy or stay clear and colorless when a drop of
silver nitrate solution is added – the less cloudy, the better. We have now filled all of
the exchange sites on the resin with H+ and removed all excess acid.
Measure the mass of the vial containing the mineral and transfer a new sample of not
more than 0.3 g to a clean, but not necessarily dry, beaker. Measure the mass of the vial
to find the exact amount of mineral that was transferred. Add about 40 mL of water to
the mineral, ensure it all dissolves, and add all of the resulting solution to the column.
Collect the eluate in a clean conical flask. Rinse the beaker with a wash bottle and add
the rinsing to the column. Run 100 mL of distilled water through the column, and
collect in the same conical flask. Keep the eluate in the conical flask, and store until you
are ready to titrate. (If you need to run a second sample through the column, separately
collect the eluates. It is not necessary to regenerate the column between samples.)

How to Analyze the Eluate

The eluate now contains as many H+ as there were positive charges in the mineral
sample. According to the equation below

each mole of NaOH will react with exactly 1 mol of H+. Because each mole of double-
positive metal ions in the mineral will produce two moles of H + ions, we can easily
calculate the moles of metal ions from the number of moles of NaOH consumed.
You have already determined the concentration of a NaOH solution by allowing it to
react with a known weight of KHP. Titrate the eluate with your standardized solution
of NaOH.

If you severely overshoot the end point, all is not lost! Add a known amount of solid
KHP, and then titrate carefully to the end point. This is known as a back titration. The
bookkeeping may be a bit more difficult, but it sure beats starting over!

38
Doing Calculations and Uncertainty Analysis

The calculation here is very similar to the calculations done in the standardization of
NaOH. See the section “Reporting your results” to get started on your Excel
calculations for this part of the experiment.

1. You should have computed the concentration of your NaOH solution and its upper
and lower limits when you were standardizing the solution (Experiment 2).
2. Compute the moles of H+ in the eluate sample from the moles of NaOH required for
neutralization. Remember to correct for any back titration. Compute the number of
moles of metal ion in the sample you used; remember that the ion exchange column
releases two H+ ions for each M2+ ion exchanged. Then calculate Mmetal the number of
moles of metal ion per gram of mineral.

1
moles M2+ (Molarity NaOH * vol. NaOH)
Mmetal = = 2
mass sample mass mineral

3. Compute upper and lower limits for the number of moles of metal ion in your sample
by following the same procedure as that in Step 2. The upper limit of Mmetal will be the
upper limit of the number of moles of metal ion divided by the lower limit of the weight
of mineral sample used. With this hint, you should also be able to work out the lower
limit.

Reporting Your Results

Set up a worksheet in Excel with the entries shown in Figure 3.3. Fill in your data in the
appropriate cell locations. For example, the net mass of mineral you used in Part B
should be entered in cell C3.

Now you are ready to work out the formula of the mineral. Use Excel formulas to do
the following calculations. When you have finished your calculations in Excel, copy and
paste the Tables into the Results section of your lab report. Also, use the Ctrl +`
command you learnt in the Excel lab to display your formulas. Make sure that the
formulas are completely visible and take a screen shot including the column and row

39
headers (i.e. A, B, C, D, etc. and 1, 2, 3, 4, etc.). Paste this screen shot into the
Calculations section of your lab report.

Figure 3.3 Excel workbook example for reporting Formula of Mineral lab data.

40
1. To obtain the formula of the mineral, compute the following:

Mwater = the number of moles of water per gram of mineral

Msulfate = the number of moles of sulfate per gram of mineral
Mmetal = the number of moles of di-positive metal ion per gram of mineral.

Calculate the upper and lower limits for all your M and G values.

41
2. Charge Balance: The correct formula must have an equal number of positive and
negative charges. If the experiment has been carried out correctly, the limits for Msulfate
and Mmetal should overlap. Msulfate should be equal to Mmetal by charge balance.

3. Water of Crystallization: To calculate the number of Waters of Crystallization (WC)

divide Mwater by your best value of Msulfate or Mmetal. Indicate in cell A23 which analysis
you used. Note that the H2O may not have an integer mole ratio to the rest of the
molecule. You also need to calculate the upper and lower limits for this value. In your
table heading, indicate the analysis you used to calculate WC, i.e. “metal” or “sulfate”.

4. If we use Gmetal to denote the number of grams of metal ion per gram of mineral, then
it is true that

Gmetal = 1 - Gsulfate - Gwater

where Gsulfate and Gwater stand for the number of grams of sulfate per gram of mineral
and the number of grams of water per gram of mineral, respectively. Compute Gmetal
and the upper and lower limits of Gmetal.

5. The relative molecular mass (RMM) of the metal ion will be simply

Gmetal
RMMmetal =
Mmetal

Calculate the upper and lower limits of the relative molecular mass of the metal ion.

For your discussion

1. Are your results consistent with each other? For example, do you have charge
balance? If not, explain why not. Discard (but still report) runs where blunders have
been made, but explain in the discussion why the run is being discarded. You may
have to choose the better value of Mmetal or Msulfate and set the other one equal to it in
calculations. If so, explain which is the better value and why.

2. If your results support one of the formulas in Table 3.1, state and explain which one,
and also any that can't be ruled out. Note that mineral samples can often be mixtures of
the same material with different amounts of water of hydration (a mixture of mirabilite
and thenardite, for example, is a reasonable result).

42
3. If your results do not support the choice of a mineral below, you should report the
formula of the mineral and the apparent atomic mass of its M2+ ion. Note that the ion
may not really be M2+. If it is M3+, your atomic mass will appear to be only two-thirds
of the true value. If it is M+, then your atomic mass is twice the true value.

4. A student taking this course finds that Msulfate is larger than Mmetal. It is known that
the value of Mmetal is the correct one. Explicitly describe what might have happened to
produce this discrepancy?

This is a long report, but when you have finished it, you will understand uncertainty
analysis, which is a useful tool for planning any scientific experiment.

Table 3.1 Some Common Sulfate Minerals

Apparent Atomic
Mineral Mass of M2+ (g/mol)
Simple Sulfates
epsomite MgSO4•7 H2O (M2+ = Mg2+) 24.31
bexahydrite MgSO4•6 H2O 24.31
leonardite MgSO4•4 H2O 24.31
mirabilite Na2SO4•10 H2O (M2+ = 2Na+) 45.96
thenardite Na2SO4 45.96
Double Sulfates
leonite K2Mg(SO4)2•4 H2O 51.28
schonite K2Mg(SO4)2•6 H2O 51.28
konyaite Na2Mg(SO4)2•5H2O 35.13
kalinite KAl(SO4)2•12 H2O 33.04

43
Experiment 4: Determination of an Equilibrium Constant

In this experiment, you will measure the value of an equilibrium constant and its
dependence on temperature. The reaction chosen is that of the dye xylenol orange with
Al3+ ions. The dye structure is shown in Figure 4.1 below. It is an interesting molecule
because it can undergo acid-base reactions and combine to form complexes with metal
ions.

Figure 4.1 The Structure of Xylenol Orange

CH2COOH CH2COOH

N N
HOOCH2C CH2 H2C CH2COOH

HO C C O
C CH HC C

C C C C
H3C C C C CH3
H H
C SO3H
HC C

HC CH
C
H

In this structural formula, only one of the many possible resonance forms is shown. The
π systems of all three rings overlap to form a continuous delocalized system, and the
electrons can migrate all over this network. This gives rise to unoccupied low-lying
electronic states and to the absorption of visible light. The compound can also undergo
significant rearrangements in acidic or basic media. (It has structural elements similar to
those of phenophthalein.)

The protons of the four -COOH groups are easily lost, and so we will think of xylenol
orange as a tetraprotic acid and abbreviate it H4Q.

44
What is the reaction you will Study?

H4Q (aq) + Al3+ (aq) QAl– (aq) + 4 H+ (aq)

Because the only colored species in this reaction are the QAl– complex and the H4Q, you
should be able to follow the reaction by monitoring one of them. You will do this by
measuring the intensity of the color of the QAl– complex.

The intensity of color is related to the concentration by Beer's Law. This relationship
and the use of the Spectronic 20, which is the instrument used in this experiment, are
discussed in the first section of Instrumentation at the end of this manual.

Measuring the Value of the Equilibrium Constant

To measure the equilibrium for the above reaction we need to be able to determine the
concentration of the QAl– molecule. Luckily, the H4Q is not the same color as the QAl–,
so we will make our observations at a wavelength of 550 nm, which is close to the
maximum absorbance of the QAl– molecule. Nevertheless, there will be some
absorbance due to the unreacted xylenol orange, and a "blank" or control must be used
to overcome this.

1. Clean three test tubes of 1 cm diameter. Pipette exactly 2.0 mL of xylenol orange into
each. The easiest way to provide suction for the small pipette required is to use a
syringe and to connect it with a small section of rubber tubing. After the xylenol
orange, pipette exactly 2.0 mL of Al3+ into the three test tubes. One of these test tubes
will remain at room temperature, at which no reaction takes place, and will be a control.
The other two test tubes will be heated in a water bath.

2. Add about 150 mL of water to a 250-mL beaker, immerse two of the test tubes, and
bring the water to the boil. Continue to boil the water for at least 5 min to allow the
equilibrium to be established. Then use a test tube holder to remove one of the test
tubes and place it in an ice bath. Using the test tube holder, place the second test tube
in a test tube rack. Use the beaker tongs to pour off the hot water into a thermocup (put
one Styrofoam cup inside another). Still using the test tube holder, transfer the test tube
from the rack to the thermocup, which will slow the cooling process. Use a
thermometer to measure the water temperature. When the water cools to about

45
90 – 85 °C, make the first measurement. Then repeat every 5°C or so, until the sample
reaches 50 °C.

3. To make a measurement, put your control test tube of xylenol orange into the
Spectronic 20 and adjust for 100% transmittance. (Double-check that the wavelength is
set at 550 nm). Pull out the test tube in the hot water bath, noting the temperature.
Wipe it dry with a paper towel, and put it into the Spectronic 20 sample holder. Read
the % transmittance of the mixture, and then re-place the test tube into the water bath.
Be careful not to bum yourself or to spill the solution into the Spectronic 20. Perform
this operation quickly to avoid the solution cooling while in the Spectronic 20.

At the end of the experiment you should have a series of measurements of the %
transmittance for at least six temperatures. You can repeat the experiment any number
of times by reheating the contents of the tube to 100°C, waiting 5 min, and letting the
tube cool slowly. Be sure to record the concentrations of the solutions used and all the
other label information.

4. The last and, in many ways, the most interesting experiment is to measure the %
transmittance of the test tube that has cooled in the ice bath. Record the color of the
solution as well.

For the Report

Set up a worksheet in Excel with the entries shown below. Fill in your data in the
appropriate cell locations. For example, your first temperature reading should go in cell
B10 and the corresponding percent transmittance in cell C10. Use as many or as few
rows as you need for your data in Table 2.

Use Excel formulas to do the following calculations. When you have finished your
calculations in Excel, copy and paste the Tables into the Results section of your lab
report. Also, use the Ctrl +` command you learnt in the Excel lab to display your
formulas. Make sure that the formulas are completely visible and take a screen shot
including the column and row headers (i.e. A, B, C, D, etc. and 1, 2, 3, 4, etc.). Paste this
screen shot into the Calculations section of your lab report.

46
 Figure 4.1 Excel worksheet example for Equilibrium data

1. Convert your % transmittance numbers to absorbance (A) by using the formula,

æ % transmittance ö
A = -log10 ç ÷
è 100 ø

The concentrations of QAl– are computed from Beer's Law.

𝐴 = 𝜀𝑐𝑙

47
The extinction coefficient,  is 25,000 L/mol cm for this compound (a very intense color,
comparable to that of permanganate). Take the path length as 0.90 cm.

2. The concentration of H+ is determined from the pH marked on the container and will
be virtually unchanged throughout the reaction.

3. The concentration of the other two species can be obtained by means of

stoichiometry:

éëAl3+ ùû = éëAl3+ ùû - éëQAl- ùû and [ H 4Q]equil = [ H 4Q]initial - éëQAl- ùû

equil initial equil equil

Remember that the initial concentrations are referring to the starting reagent
concentrations in the test tubes. These concentrations are half those marked on the
bottles because of dilution.

3. From these equilibrium concentrations, compute the value of the equilibrium

constant (K) at each temperature.

éëQAl– ùûéëH + ùû
4

K=
[ H 4Q] éëAl3+ ùû

4. The fact that the equilibrium constant depends on temperature is useful, because it
allows you to measure ∆G°, ∆H°, and ∆S° for the reaction. You can easily obtain the
equilibrium constant from the concentrations. The relationship between ∆G° and K is:

DG° = -RT ln K

Therefore, you can calculate ∆G° at any temperature if the value of the equilibrium
constant K is known.

It is also true that

∆G° = ∆H° - T∆S°

If these two equations are combined, we obtain

48
 -RT ln K = ∆H° - T∆S°

This equation can be rearranged very slightly to yield

DH° æ 1 ö DS°
ln K = - ç ÷+
R èTø R

which has the form of an equation for a straight line:

y = mx + b

where m is the slope and b is the intercept. Hence, if one plots ln K on the y axis
versus 1/T on the x axis, the slope of the resulting straight line will be -∆H°/R
and its intercept will be ∆S°/R. Use Excel to plot your ln K versus 1/T data excluding
the tube that was rapidly cooled in ice water. Include a linear best-fit line and display
the equation of the line on your graph. Calculate and report the ∆H° and ∆S° values
derived from your data.

Note that R = 8.314 J/mol-deg and that T must be in Kelvins (°C + 273.15). This
argument does assume that ∆H° and ∆S° are independent of temperature over the small
range of measurement. For extended discussions of the meaning of ∆G° and ∆H°, refer
to your textbook.

Discussion Questions

In the discussion part of your lab report, consider the following questions:

1. Compute the equilibrium constant of the tube that has been quickly cooled. Which
of the equilibrium constants measured in Step 3 does this seem closest to, and what was
the corresponding temperature in Step 3? How do you account for the fact that this
temperature is much higher than that of ice water?

2. Is the sign of ∆H° correct? (Recall that the reaction seems to be displaced toward
QAl– at high temperatures.)

49
Practical Exam I: Percent Sodium Oxalate in an Unknown

The practical exam provides an effective test of lab technique and skill. Luck actually
plays a very small role, and chance always favors the prepared mind. Use your best
technique, and demonstrate here that you are now at home in the world of precise
measurement.

Rules for the Practical Exam

1. You may not talk to one another, compare results, or share calculators. The exam is
"closed-book," unless otherwise announced, but you may bring your lab notebook, and
the report form.

2. The teaching assistant who is present is a timekeeper and safety monitor and will not
answer questions about end points, which values to discard, or other such decisions.
You should make these judgments yourself. The teaching assistant may help you if you
have an equipment problem beyond what you might reasonably be expected to cope
with.

3. Eye protection and proper attire are required at all times. You will be asked to leave
the lab and therefore fail the exam if you do not wear them.

4. To obtain a sample, you must turn in a signed receipt. You will not be issued
another sample if the first one is damaged, lost, or destroyed.

5. Come on time. Once you start the exam, you may not come again on another day.
(Time is not normally a problem for most students taking this exam.)

6. No visitors will be admitted to the rooms where the exam is held.

7. Bring a working calculator. If you use your report form, you will not be penalized
for mathematical errors, but you are the person best qualified to choose the best value.

During the lab session scheduled the previous week, you will make the required
solutions and do other essential chores. We suggest that on the day of the exam you
copy a set of explicit directions into your notebook. There will be no instructions on the
Whiteboard.

50
The Problem You are to Solve

You will be given a sample containing an unknown amount of sodium oxalate

(Na2C2O4). You will be expected to tell us the percentage of Na2C2O4 very accurately by
doing a titration with the strong oxidizing agent KMnO4. The balanced equation for the
net reaction is

5 C2O42- + 2 MnO4– + 16 H+ 10 CO2 + 2 Mn2+ + 8 H2O

This reaction can be used for titration only if the solution temperature is at least 70 °C to
90 °C.

The most common causes of errors seem to be:

1. Failing to understand the instructions.

2. Preparing your KMnO4 solution poorly. This category breaks down into a number of
sub-problems, such as not mixing the solution thoroughly. The average student
seriously underestimates the shaking required to mix things. The solution must be
absolutely uniform – it is impossible to shake it too much.

3. Contaminating the primary standard, the pure solid Na2C2O4.

4. Mixing up records. (This is inexcusable, but it keeps happening. Make sure it does
not happen to you.)

5. Making blunders in the use of, for example, the buret and the balance. The practical
exam is extremely efficient at finding people who, for example, do not know how to
read the balance correctly. If you have any lingering doubts, ask your teaching
assistant, even if you think you really ought to know.

6. Averaging good runs with those in which blunders occurred. Averaging does not
reduce systematic errors; it only means that good data are spoiled. Only average your
results if you are reasonably sure that no blunders occurred that could affect them. It is
far better to have one good standardization and one good titration of the unknown than
to have three poor runs.

51
Preparing the Solution

CAUTION: This experiment involves two dangerous chemicals. One is potassium

permanganate, KMnO4, which oxidizes any organic matter it comes in contact with,
papers, clothes, and skin. If you spill any on your skin, wash it off with large
amounts of water. Permanganate stains of glassware can be removed with a dilute
sodium bisulfate solution, NaHSO3.

Also, you will be using 3M sulfuric acid. This attack skin and clothes. If any acid is
spilled on your skin or clothes, wash immediately with generous amounts of water.

What you do today affects your results. Be sure to complete the following:

Preparation of the KMnO4 solution.

You should prepare 400 mL of KMnO4 solution. Measure out between 2.000 and
4.000 g of KMnO4. This can be done on a beam balance.

Dissolve the KMnO4 in a 600 mL beaker with 400 mL of deionized H2O (this can be
measured with a graduated cylinder). Cover the beaker with a watch glass; warm it,
but do not boil, stirring occasionally. Allow the solution to cool until it is comfortable to
handle, and then cool it further by running cold water over the outside. Pour the
KMnO4 solution into a glass reagent bottle for storage. Solutions of KMnO4 deteriorate,
and for precise work the concentration must be determined on the day of use. Shake
thoroughly for one full minute before using to fill a clean burette.

Standardization of the KMnO4 solution.

Measure between 0.3000 - 0.5000 g of solid Sodium Oxalate into a conical flask. Record
the exact weight. Dissolve the solid in 25 – 35 mL of 3M H2SO4. Raise the temperature
of the mixture being titrated to 70°C to 90°C to speed the reaction, but do not let it boil
lest some be lost by spattering. If you put a thermometer into the mixture, be sure to
rinse it into the mixture being titrated. Titrate with your KMnO4 solution. The end
point is the faintest of pinks. When you are done, do not put any of the KMnO4 solution
in your buret back into your bottle of KMnO4.

52
 SAVE THE KMnO4 SOLUTION FOR THE EXAM
On the day before the practical exam, reread the section of the book called “How to Be
Successful in Lab” so that you recall all of the special tricks of titration.

Doing the Oxalate Analysis (Exam)

You will have 2 hrs and 30 min to do this part.

1. Obtain an unknown sample from the TA in your lab room. A signed receipt is
required.

2. Because it gradually deteriorates, the KMnO4 solution must be standardized again on

the day it is to be used. Shake the solution vigorously for one full minute before
beginning. Standardize the solution against oxalate as described above. Do not forget
to heat the solution.

3. For the titration of the unknown, place about 1.0000 g of the unknown solid in a
conical flask, recording the exact mass. Measure out one sample at a time, so that if too
much or too little KMnO4 is used, you can adjust the next sample size next time to be
more convenient. Dissolve the unknown in at least 25 mL of 3M H2SO4. You may wish
to heat it to speed up dissolution. Remember, the reaction occurs rapidly only when the
solution is hot, so you will have to heat until the temperature of the solution is 70 °C to
90 °C before titrating.

4. Ideally, you should do three standardizations and three titrations. The ratio of
KMnO4 to Na2C2O4 in your standardization titration should not be drastically different
from that on the dry run day. Work with deliberate speed and do not waste time, but it
is much preferred to obtain one good pair of runs than three poor ones.

5. When "time" is called, stop work and complete the calculations on the report form.
You may choose the mean, the median, or the best value, or you may just guess. If your
answer for oxalate content is not between 10% and 40%, you have probably made a
mathematical error. Your grade will be based solely on how close your number is to the
correct value of the unknown. Give some thought to the choice of mean, median, or
best value.

6. Avoid the following errors:

53
 a) Mis-reading your buret.
b) Forgetting to heat the solution (end point appears sluggish).
c) Forgetting to add H2SO4 where needed (end point brownish).

7. Before you leave, be sure to clean your work area, wiping up any spills. You will
dispose of the solutions during the Check-out period. Keep the sample vials until then.

54
INSTRUMENTATION: USING THE SPECTRONIC 20

The Bausch and Lomb Spectronic 20 (see Fig. 5.1) is the "workhorse" instrument for all
measurements involving light. It works in the wavelength region of 380 to 620 nm
without modification. To use this instrument, begin by locating the controls. To use the
Spectronic 20, follow these instructions:

1. Switch on the machine. Let it warm up for at least 10 min. You will need two
solutions, a blank, for correcting for the solvent readings, and the sample
solution to be measured.
2. Select the desired wavelength by using the wavelength control, the knob on
top of the instrument.
3. Set the percent transmittance (top scale on the meter) to zero, using the zero
control.
4. Place a cuvette (or test tube) filled with the appropriate blank in the sample
holder. Close the cover.
5. Use the 100 % T control to set the needle to 100 % transmittance. This adjusts
for the transmittance of the solvent, test tube, and so forth.
6. Remove the blank, and close the cover over the sample holder. The needle
should swing back to 0 % transmittance. If it does not, repeat procedure all over
again.

Figure 5.1: A Spectronic 20

The instrument is now correctly calibrated, but for one particular wavelength only. To
take a reading, place a cuvette containing your sample in the sample holder, close the

55
cover, and record the % transmittance after the needle has settled down. The cuvette
must be free of fingerprints, bubbles, and other dirt.

When you are using the Spectronic 20, keep the test tube or cuvette clean; avoid leaving
fingerprints on the bottom part where the light passes through. There should be no air
bubbles on the inside, and solutions with suspended material will result in odd
readings.

The cuvette is cylindrical and therefore acts as a lens, focusing the light to some extent.
The cuvette should therefore be lined up in the same way each time. There is a mark on
some cuvettes, which can be lined up with a line on the cell holder. If there is no mark,
make a small one at the top of the tube using a wax pencil.

The calibration with the blank must be redone at each new wavelength and should be
repeated every few minutes, even at the same wavelength, to compensate for any drift
in the electronics.

Remove the cuvette/test tubes in order to fill them. Water and electricity do not mix!

How the Spectronic 20 Works

You will be measuring the amount of light absorbed at a chosen wavelength. The
Spectronic 20 is a typical absorption spectrophotometer, and it has the following basic
parts:

1. A source of light. For the Spectronic 20, this is a tungsten lamp. White light
comes out of the bulb, and lenses focus it into a narrow, parallel beam.
2. A monochromator. This is a device used to break up the light into several
wavelengths and to block off all but the wavelength of interest. In your
instrument, the light is broken up by a diffraction grating and sorted by an exit
slit, which stops all but one wavelength band.
3. A cell holder to hold a cuvette or sample test tube. In the Spectronic 20 there is an
occluder to prevent light from passing through if there is no sample in the holder.
4. A photocell or other device used to "see" the light and to give a numerical value to its
intensity. The phototube will measure all the light remaining after the sample has
done the absorbing.

56
All spectrophotometers have the same basic parts, but obviously different sources of
radiation and types of receptors are needed for different regions of the electromagnetic
spectrum. One of the reasons for taking time to understand the Spectronic 20 is that
once this instrument is understood, mastery of more complicated but basically similar
instruments is easy.

How the Spectronic 20 Controls Do Their Job

The wavelength controller adjusts the position of the diffraction grating so that different
colors of light are selected by the slit.

The zero control adjusts the electronics. With the sample compartment cover down and
no sample, this should be adjusted until the meter reads 0 for % transmittance. This
control adjusts for the so-called dark current, the current transmitted by the photocell in
the dark.

The 100 % T control, a knob on the right, controls the amount of light output. A
mechanical linkage is used to drive a wedge into the light beam. This should be
adjusted so that with a test tube full of solvent in the sample holder, the transmittance is
100 %. This allows the operator to correct for any stray absorbance resulting from the
solvent.

COLOR AND SPECTROSCOPY

When various wavelengths of light enter the eye, we see different colors. The rainbow
is an illustration of a spectrum, in which white light is sorted into its various component
wavelengths, each of which appears as a different color. Such an effect can also be
produced by a prism or diffraction grating.

The range of wavelengths visible as colors for humans is about 700 nm (nanometers,
where 1 nm = 10–9 m) to about 380 nm. It is interesting that some animals can see colors
in the wavelength region beyond violet (ultraviolet) or in the region beyond the red end
of the spectrum (infrared). Humans have to rely on sophisticated instruments to make
observations in these regions of the electromagnetic spectrum.

57
The color of light transmitted by a solution or reflected by a surface is the light that
remains after some colors have been preferentially absorbed. Chemists are interested in
the region at which light is absorbed, because this can supply information about the
structure of the molecule.

We therefore need to know what wavelength is absorbed most preferentially and also
the intensity of the absorption. The wavelength of absorption is therefore related to the
energy of the light being absorbed by the molecule. Thus, the color of the absorbed
light provides direct information about the kind of molecular transition or the kind of
molecule doing the absorbing. The intensity of absorption is related partly to the type
of molecule, but it also depends on other variables. This section first looks at the color
alone.

The Relationship of Color and Wavelength

In deciding what color something is you have to distinguish between objects that emit
light and objects that reflect (or transmit) light. A Bunsen burner flame is blue because
the combustion reaction products emit blue light. For such objects, the relationship
between color and wavelength is the same as for sunlight dispersed by a prism. The
solutions you will use are actually involved in the reverse process; instead of emitting
light of a certain wavelength, , they absorb light at wavelength, , and transmit the
rest of the light. So a solution of CuSO4 held up to a light appears blue because the Cu2+
ion absorbs yellow light and transmits the blue light, which is not absorbed. You can
figure out what color light is absorbed if you know what color is transmitted
(complementary colors) using Table 5.1.

TABLE 5.1: Relationship Between the Wavelength of Light Absorbed and the Color
You See

Light Absorbed
Wavelength (nm) Color Color You See
400-440 violet green-yellow
440-480 blue yellow
480-490 green-blue orange
490-500 blue-green red
500-560 green purple
560-580 yellow-green violet

58
 580-600 yellow blue
600-610 orange green-blue
610-750 red blue-green

The experiment you will do uses solutions that absorb light rather than emit light. The 
of the absorbed light is the wavelength of interest to chemists, because it can provide
clues about molecular structure.

Our instrument, the Spectronic 20, is calibrated in nanometers (nm), which are
wavelength units. However, the wavelength may also be expressed in Angstrom units
(Å), which are equal to 10–10 m. Also, infrared workers frequently use cm–1 (the
reciprocal of wavelength). This latter unit can be thought of as wave crests per cm and is
really an energy unit.

The Intensity of Absorption

The intensity of the color will depend on the following variables: (1) the kind of
molecule doing the absorbing, (2) the concentration, and (3) the path length that the
light passes through. To make the idea about color intensity more concrete, you can
define a quantity related to these three variables and call it absorbance, A.

𝐴 = 𝜀𝑐𝑙

This equation says that absorbance is proportional to path length l (if you double the
length of the path of light, you double the opportunities for it to be absorbed), and
proportional to concentration c (doubling the concentration creates twice as many
absorbing centers). To make the units work and to adjust for the type of substance
doing the absorbing, use ε, the extinction coefficient. The relationship is known as the
Beer-Lambert Law or Beer's Law.

This relationship can be used in many ways. If you know the absorbance for a given
concentration of a substance (at a given wavelength), then the absorbance of an
unknown solution can provide you with the concentration of the unknown, if you are
careful to use the same cell and wavelength.

If you know the absorbance, the path length, and the concentration of a substance, it is
easy to compute the extinction coefficient, and this can provide important clues to the

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molecular structures involved in the transition. The extinction coefficient depends, of
course, on the wavelength, but otherwise it is a property of the molecule involved.

If the concentration is in stated moles per liter and the path length is in centimeters, the
extinction coefficient will be in liters per mole-centimeter.
The Units of Color Intensity

The meter or chart recorder supplies the intensity of absorption at a given wavelength.
It is calibrated in either or both of the two following ways:

1. Transmittance. This is the fraction of the initial number of photons that pass
through the sample without being absorbed. (Sometimes the transmittance is
expressed as a percentage.)
2. Absorbance. This is the negative logarithm of the transmittance (expressing the
latter as a fraction). It is unitless. Absorbance and optical density (OD) as the
biochemists call it) are the same thing.

The relationship between absorbance A and transmittance T is

A = – log10 T

where T is expressed as a fraction. The following example makes this clearer:

EXAMPLE: A student records a transmittance of 30 percent. What will be the

transmittance if the concentration of the solution is doubled?

Solution: Express 30 percent as a fraction, or 0.30, and compute the corresponding

absorbance,
A = – log(0.30) = 0.52

If the concentration is doubled, the absorbance is doubled (from Beer's' Law). Hence,
the new solution will have an absorbance of 1.04, and a transmittance of 9 percent.

60
Mathematical Operations

This part is largely concerned with uncertainty calculations. You will need to master
the first section to complete most of the lab reports, but the second and third sections
may well be assigned by your professor to deepen your understanding of this topic and
its applications.

If you have had to struggle with uncertainty in a previous lab course, fear not. The
method presented here is a lot simpler, and it works well enough for most student lab
work (and for a good deal of real scientific work as well.) Students who had trouble
with traditional methods can easily cope with uncertainty when it is presented in this
new way, so take heart!

A. CALCULATING UNCERTAINTY BY THE WORST CASE METHOD

There are two sorts of problems with measurements. The first kind is that of systematic
error, the situation in which one is measuring not quite what one supposes, because of,
for example, defects in instruments or technique. Such systematic errors can be
controlled only by improving the design of experiments.

This section discusses the other sort of ambiguity in data, the intrinsic uncertainty due to
the limitations of the instruments. It is assumed here that the desired quantity is in fact
being measured. However, the question is asked: how reproducible would the
measurement be if it were repeated in the same way many times? This reproducibility
or precision is of major importance in planning experiments.

Systematic errors and uncertainties differ in one crucial way. There is no way that
systematic errors can average out. If, for example, a sample from a gravimetric
experiment is not sufficiently dried before measuring the mass, the student can measure
the mass one hundred times and the problem will not be cured. However, if a sample is
correctly prepared, averaging more mass measurements will produce a result of greater
precision.

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A beginning student has far too much faith in averaging. If the measurements being
averaged contain repetitions of the same systematic errors, the result cannot be purified
by running it through the calculator!

Many classic textbooks draw a distinction between precision (the degree of clustering)
and accuracy (the absence of systematic error). Look at Fig. 6.1 showing a bear target
being shot by a marksman.

FIGURE 6.1: The Difference Between Precision and Accuracy

On the average, the bear is dead. You can average, but it does not help.
(Accuracy, no precision) (Precision, no accuracy)

Computing Uncertainties

Every measurement is uncertain in that it probably cannot be exactly reproduced a

second time. Uncertainty is a technical term for the reproducibility of the measurement.

If, for example, you measure the mass of a copper penny on a balance five times, you
will probably observe some variation in the last decimal place. Such a sequence of
results might be 3.0110 g, 3.0114 g, 3.0120 g, 3.0111 g, and 3.0115 g. The average value is
about 3.0115 g, but the range of values is at least ± 0.0005 g from that value. The
number ± 0.0005 is called the absolute uncertainty of the measurement. Clearly, the real
value (whatever that is) is somewhere between 3.0110 g and 3.0120 g. These two values
are referred to as worst cases or the upper and lower limits.

Similarly, for any other instrument there is a range of absolute uncertainty in a

measurement related to its observed reproducibility. This uncertainty is usually based

62
on the half-increment rule where the uncertainty is half of the smallest increment you
can measure. Some are given below, for the most common models of instruments in
student labs.

buret ± 0.05 mL in any single reading.

balance ± 0.0005 g in any single measurement.
360° thermometer ± half the difference between the smallest graduations.

The National Bureau of Standards (NBS) sets the following standards for absolute
uncertainty tolerable in Class A glassware (Tables 6.1 and 6.2):

TABLE 6.1: NBS Specifications for Volumetric Flasks

Capacity Tolerance Common Tolerance Class A

10 mL ± 0.04 mL ± 0.02 mL
50 mL ± 0.10 mL ± 0.05 mL
100 mL ± 0.16 m ± 0.08 mL
250 mL ± 0.24 mL ± 0.12 mL
500 mL ± 0.30 mL ± 0.15 mL

TABLE 6.2: NBS Specifications for Class A Pipettes

Capacity Tolerance, Transfer Tolerance, Measuring

1 mL ± 0.006 mL ± 0.01 mL
2 mL ± 0.006 mL ± 0.01 mL
5 mL ± 0.01mL ± 0.02 mL
10 mL ± 0.02 mL ± 0.03 mL
25 mL ± 0.03 mL ± 0.05 mL

When you are confronted with a new instrument and need uncertainty information, it is
sensible to try repeating the same measurement until some idea of the reproducibility is

63
evident. Then it is easy to choose reasonable values for worst cases. (There is, of
course, some judgment involved.)

Combining Measurements and Computing Worst Cases

The difficult part of performing uncertainty calculations is in the combining of different

sorts of measurements to reach a conclusion. However, by writing down the upper and
lower limits of the individual measurements, it usually becomes clear how these can be
combined to provide worst cases for the results. To save time, remember the following
rules:

1. If the main calculation requires multiplying numbers together or adding

numbers together, multiply or add upper limits to find upper limits, and
multiply or add lower limits to obtain lower limits.

2. Always divide opposite limits. Put an upper limit over a lower limit to obtain
an upper limit. Place a lower limit on top and an upper limit on the bottom, and
the ratio will be the lower limit. If you think about ratios for a moment, you see
why this also is obvious. As long as you remember to combine the opposite
limits, things will work out fine, because it will be quite clear from the values
themselves which limit of the quotient is which.

3. Subtract opposite limits. Again, if you remember to combine opposite limits, it

will be quite clear which limit of the difference is which.

4. A corollary: If subtracting two measurements on the same instrument to obtain

a net weight, or net volume, the absolute uncertainty in the net value will be
twice the absolute uncertainty of the individual measurements.

An example shows this very easily: A student measures a value of 5.00 mL using a
buret accurate to ± 0.05 mL to deliver the volume. Two readings are taken: 4.92 mL
and 9.92 mL (Table 6.3). The volume delivered is 5.00 mL, but what is the range of
uncertainty?

64
 TABLE 6.3: Sample Buret Readings
Lower Limit Volume Upper Limit
Final measurement (mL) 9.87 9.92 9.97
Initial measurement (mL) 4.87 4.92 4.97

Worst cases of the difference are as follows:

Upper Limit: 9.97 – 4.87 = 5.10 mL

Lower Limit: 9.87 – 4.97 = 4.90 mL

Hence, the net value delivered is 5.00 ± 0.10 mL.

Some Worst Case Calculations

This section contains a few examples of uncertainty analysis in action.

Calculating Uncertainty in a Weighing Experiment

The energy content of coal, and therefore its price, depends on the water content.
Therefore, it is necessary to determine this content accurately. The coal is placed in a
crucible and heated in an oven so that the water is driven off. Let us assume that the
coal is about 10 percent water and we are using a 0.8000 g sample.

Step 1. Obtain the net mass of wet Coal.

Lower Limit Weight Upper Limit
Mass of wet coal and crucible 20.7995g 20.8000g 20.8005g
Mass of crucible empty ("tare weight") 19.9995g 20.0000g 20.0005g
Net mass of wet coal 0.7990g 0.8000g 0.8010g

65
These upper and lower limits are calculated in exactly the same way as in the buret
example:

Upper limit: 20.8005 g – 19.9995 g = 0.8010 g

Lower limit: 20.7995 g – 20.0005 g = 0.7990 g

So, the net mass of wet coal is 0.8000 ± 0.0010 g.

Step 2. Obtain the mass loss of coal

Mass of wet coal and crucible 20.7995 g 20.8000 g 20.8005 g

Mass of dry coal and crucible 20.7195 g 20.7200 g 20.7215 g
Mass loss 0.0790 g 0.0800 g 0.0810 g
(again, computed as above) (or 0.0800 ± 0.0010 g)

Step 3. Obtain the percentage of mass loss. The percentage of H2O in the coal
will

mass loss
percentage = × 100
original mass
One worst case will be

upper limit of mass loss 0.0810

= × 100 = × 100 = 10.14 %
lower limit of original mass 0.7990

The other worst case will be

lower limit of mass loss 0.0790

= × 100 = × 100 = 9.86 %
upper limit of original mass 0.8010

Hence, the true percentage of water lost lies between 10.14 percent and 9.86 percent.

This problem could be simplified by realizing that the "net" quantity rule (the corollary,
Rule 4) applies to Steps 1 and 2.

How to Calculate Uncertainty in a Concentration

66
A solution is made up in an l00 mL volumetric flask. The substance has a molecular
mass of 120.0 g/mol, and 2.6754 g are measured out. What is the uncertainty in the
concentration?

2.6754 g
Concentration = g = 0.2229 𝑀
(0.10000 L)(120.0 )
mol

The mass is determined by measuring the mass of a vial containing the solid, then
transferring the solid quantitatively to the flask, and measuring the mass of the vial.
The absolute uncertainty in each mass measurement is ± 0.0005 g. The mass is a net
mass, so the absolute uncertainty of the net mass is ± 0.0010 g (by Rule 4).
The flask is 100.00 mL nominally and has an absolute uncertainty of ± 0.08 mL (if it is
Class A). The volume limits, therefore, are 99.92 mL and 100.08 mL. Combining the
upper limit of weight with the lower limit of volume provides the upper limit of
concentration.

2.6764 g
Upper limit = g = 0.2232 𝑀
(0.09992 L)(120.0 )
mol

2.6744 g
Lower limit = g = 0.2227 𝑀
(0.10008 L)(120.0 )
mol

The last step of this example illustrates the division rule about division of worst cases.

As a final point, in this course we do not require you to consider human uncertainty in
your worst case calculations. Human uncertainty is typically larger than instrumental
uncertainty and can be experimentally determined. In other courses, you may be
required to consider the effect of human uncertainty on your results.

Problems for You to Solve

1. Jo Superior is a student at a college where the balances are accurate only to ± 0.005 g.
Into a crucible with a mass of 20.100 g empty, she puts some copper powder and
measures the mass, obtaining a reading of 21.100 g. An excess of sulfur is added, and
then the mixture is strongly heated under a hood. The excess sulfur vaporizes, leaving

67
a nonvolatile compound of copper and sulfur in the crucible. The mass of the crucible
and compound is 21.554 g. The atomic mass of copper is 63.54g/mol; atomic mass of
sulfur is 32.06 g/mol.

Compute the upper and lower limits for the ratio of moles of sulfur to moles of copper.

2. A titration of 0.2686 g of an unknown acid HX requires 23.06 mL of NaOH solution.

The concentration limits of the base solution are 0.0872 M and 0.0884 M. What are the
upper and lower limits for the molecular mass of the HX?

3. A l0 mL Class A pipette is used to deliver a sample of solution of unknown acid HX,

which is titrated with 23.06 mL of NaOH, the concentration of which can be taken as
exactly 0. 01000 M. What are the upper and lower limits for the concentration of the HX
solution?

B. A SHORT CUT IN UNCERTAINTY ANALYSIS

In the previous exercises, you have often found the need to calculate worst cases for
results obtained by multiplying and dividing measurements (with known worst cases)
and constants. This method tends to be laborious, and so the following short cut is
offered.

Calculating Relative Uncertainty

Relative uncertainty is defined as the ratio of the absolute uncertainty (defined in the
preceding section) to the quantity being measured.

absolute uncertainty
𝑅𝑈 = × 100
the measurment itself

This is usually expressed as a percentage (which explains the factor of 100). It tells you
what percentage of the measurement is uncertain. This is very useful, because although
absolute uncertainty may not be very meaningful it is obvious that a measurement
having a 1 percent relative uncertainty is better than one having a 10 percent relative
uncertainty.

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Given the formula above, it is easy to compute relative uncertainty in any specific case.
Note that whereas the absolute uncertainty depends on the instrument, the relative
uncertainty depends on the size of a measurement. For example, if you weigh 1.0000 g
by difference, our absolute uncertainty will be ± 0.0010 g. This absolute uncertainty is
the same if you measure 0.1000 g. However, the relative uncertainty is different:

0.0010 g
for 1.0 g 𝑅𝑈 = × 100 = 0.1 %
1.0000 g

0.0010 g
for 0.1 g 𝑅𝑈 = × 100 = 1.0 %
0.1000 g

If the relative uncertainty is calculated correctly, it should be unitless. (The absolute

uncertainty and the measurement itself will always have the same units.)

Using a Short Cut

If you are computing Y, where Y is derived from measurements by multiplying or

dividing,

Y = kABCDE

and A, B, C, D, E are measurements and k is a constant, then it is approximately true

that RU of Y = sum of relative uncertainties of A through E.

Then, if you multiply Y itself by the relative uncertainty of Y, you obtain the absolute
uncertainty of Y and can construct worst case upper and lower limits. In summary,
then, to perform this trick do the following:

1. Convert absolute uncertainties to relative uncertainties for each of the

measurements, to be multiplied or divided.

2. Add all of the relative uncertainties.

3. Compute the absolute uncertainty of the result by multiplying the relative

uncertainty of the result by the result itself.

69
 4. Construct worst case limits for the result.

Understanding Why This Short Cut is Useful

Not only does this short cut save time, it pinpoints the weakest link in the chain of
measurements being used to lead to a conclusion, because this one will have the highest
relative uncertainty.

The result you obtain may not be exactly identical to that from the worst case method,
but it will probably differ only slightly. Because absolute uncertainties are often just
estimates anyway, you do not need to worry.

Remember the limitation of this trick: All measurements must be related to the final
derived value by multiplication or division, or by multiplication or division by a
constant. This short cut does not work for addition or subtraction.

An Example Uncertainty in a Standardization

A student finds that 0.5089 g of potassium acid phthalate exactly neutralizes 23.06 mL
of a NaOH solution of unknown concentration.

Step 1. Calculate the concentration itself. The number of moles of potassium acid
phthalate used is

0.5089 g
= 2.492 × 10−3 mol
204.22 g/mol

Since each mole of this substance reacts with the same number of moles of NaOH,
there must be 2.492 × 10–3 mol of NaOH in 23.06 mL of solution. So, the
concentration will be
2.492 × 10−3 mol mol
= 0.1080
0.02306 L L

Step 2. Compute relative uncertainties. The potassium acid phthalate was weighed by
difference; hence, the uncertainty in each weighing is ± 0.0005 g, and the total
absolute uncertainty is ± 0.0010 g. Thus, the relative uncertainty of the weight of
potassium acid phthalate is

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 0.0010 g
× 100 = 0.20%
0.5089 g

This is also the relative uncertainty of the number of moles of potassium acid
phthalate, and, therefore, of the number of moles of NaOH (since we assume that
there is no uncertainty in the molecular weights).

The volume of NaOH is measured by difference. Because the initial buret reading is
uncertain by ± 0.05 mL and the final reading by ± 0.05 mL, the total absolute
uncertainty is ± 0.10 mL. This gives the relative uncertainty on the volume as

0.10 mL
± = 0.43 %
23.06 mL

Step 3. Add the relative uncertainties. The relative uncertainty of the NaOH
concentrations will be given by

RU of NaOH concentration = RU of NaOH mol + RU of NaOH vol

RU of NaOH concentration = 0.20% + 0.43% = 0.63%

Step 4. Convert the RU of the result back to an absolute uncertainty. The absolute
uncertainty will clearly be

0.63%
( ) (0.1080 𝑀) = ± 0.0007𝑀
100

Step 5. Construct worst case limits. Thus, the true value of the NaOH lies between
0.1073 M and 0.1087 M (0.1080 M ± 0.0007 M).

71
Reporting Lab Results

The point of writing a lab report is to summarize experimental results in a compact

form, to draw conclusions, and to communicate the results to others. Each project in
this course revolves around certain scientific questions. By writing the report, you are
using your data to answer these questions. In the process, you will gain a mastery of
the relevant theory and also learn some data reduction techniques of general scientific
applicability.

Reports need not be typed or elegant. But the information should be presented in a clear
and logical format. You are urged to layout your data and calculations in tabular form,
wherever possible, and graphs must follow the standard conventions of the scientific
journals. In general, however, you may exercise any amount of ingenuity that you
want.

All the projects in this manual have explicit instructions as to what needs to be reported.
Unless your instructor specifies differently, all reports must contain the following
general sections:

1. Title page with your name, your teaching assistant's name, the date, and your
unknown number (if applicable).

2. Purpose. In 50 words or less, state the molecular question that the lab is trying
to answer.

3. Procedure. Normally you can simply cite this manual, giving page numbers;
however, if changes were made-even by the instructor's direction you should
mention them.

4. Results. Layout your data in tabular form, and also show one sample for each
new calculation. You need only tabulate answers, if the same calculation is
repeated. The final results should be shown together with their worst case limits
or absolute uncertainties. The final results should also be stated to an
appropriate number of decimal places (that is, it is foolish to report a value as
8.147 if the real range is from 8.11 to 8.18). Units should be attached. This helps
keep you from making blunders in arithmetic.

72
 5. Discussion. This should contain answers to the specific questions being asked
in the manual. Each project description contains a number of "leading questions"
to start your thinking about what to write in the discussion. Please limit yourself
to a few hundred words.

Using Scientific Notation and Significant Figures

It is useful to report numbers with scientific notation; that is, instead of 0.0203, report
2.03 × 10-2. Realize also that the number of places reported matters, that is, 2.030 implies
precision to the last place, and 2.0 implies only that the number is between 1.9 and 2.1.

The digits in a number that are known with certainty, plus one more, are customarily
reported. These are known as significant figures. Thus, the number 2.03 × 10-2 implies
that the value is between 2.02 × 10-2 and 2.04 × 10-2 (if no uncertainty is explicitly stated).

Although there are formal systems for keeping track of significant figures, if you
understand what it means to be "significant," you will never fall into the trap of
reporting 8.6412 for a number that is somewhere between 8.63 and 8.65.

Units should be attached to all numbers that need them, especially final results.

How to Prepare Graphs

A number of lab reports require that you prepare graphs. Over the years, scientific
journals have developed rigid standards for graphs. Your work must conform to these
standards, so that you acquire good habits.

The standards are as follows:

1. The variable being measured (dependent variable) is on the y-axis (vertically).

The variable being adjusted by the experimenter (independent variable) is on the
x-axis. Axes should be labeled, with the unit in parentheses.

2. Points must be large enough to be seen, and different series of data may be
indicated only by shape and symbol, not by color, and a key or caption should be
provided.

73
 3. Graphs must include a descriptive title explaining what the graph means.

Do not connect the points with straight lines. Instead, let the shape of the line reflect the
underlying relationship. A linear relationship calls for a straight line; curves may be
appropriate if the underlying relationship is more complicated. Computer generated
graphs are acceptable and preferred.

How to Write the Discussion

Most students seem to breeze through the calculations but are stumped by the
discussion part of the lab report. This section contains a report of one experiment, and a
sample discussion, to provide an idea of the possibilities.

Reporting the Data and Calculations of a Sample Experiment

Students were asked to identify the metal in a cylindrical slug by measuring the volume
and mass, and computing the density. The following are the data of the world famous
A Student:
mass of slug = 17.0776 g ± 0.001 g

Volume measurements were done by dropping the slug into a buret partially filled with
H2O and noting the initial and final volume measurements. The volume is therefore a
"net" measurement recorded in the student's notebook as follows:

volume measurement of slug = 40.03 - 34.07 mL

net volume = 5.96 ± 0.10 mL

The data are tabulated in the report in Table 7.1:

Table 7.1: Identification of an Unknown Slug Data

Lower Limit Measurement Upper Limit

Mass of slug (g) 17.0766 17.0776 17.0786
volume of slug (mL) 5.86 5.96 6.06
density of slug (g/mL) 2.82 2.87 2.91

Do not worry at this point about how the uncertainty limits are derived; this is
explained in the chapter on mathematical operations.

74
Discussing the Data of the Sample Experiment

The student's discussion, covering the above data, appears as follows:

The measured density was 2.87 g/mL with the "true" answer in the range of 2.82 to
2.91 g/mL. This density is closer to that of aluminum (2.6989 g/mL) than to any other
metallic element. However, the density of the aluminum is outside the range of
uncertainty, and we therefore conclude that

1. The sample is not pure aluminum (possibly an alloy of aluminum with a denser
material?)
or
2. There may be an unnoticed systematic error in the measurement. Since the weight
measurement was made on an analytical balance, this could be wrong only if the balance
were improperly calibrated, a remote possibility.

The error, therefore, probably lies in the volume measurement if the hypothesis of
systematic error is correct. The volume would have to appear too small. This could
occur, for example, if the act of dropping the slug into the buret splashed water up onto
the sides, where beads would cling, and thus the rise in the water level would be less than
expected. This was not observed by the experimenter, and the buret was clean enough so
that such beads of water ran down immediately.

Given the extreme simplicity of the experiment, Hypothesis 1 seems more likely.

This discussion is a good one because

1. The writer does not jump to conclusions. Just because the value of the density is close
to aluminum does not make the plug aluminum!

2. The writer is not bothered by the fact that his or her results are not quite what was
expected. The discrepancy is simply patiently explained.

3. The writer is specific and does not appeal to vague arguments like "human error,"
"inadequate instruments," or "defective technique." The argument about splashing
proceeds in the proper direction. The writer shows why splashing might result in a

75
lower volume reading and why this would result in a density that is too high. The
writer argues intelligently about what is the most likely explanation of the findings.

76