Principles of Chemistry I

CHEM 101

Laboratory Manual

2023-2024
 Safety and Liability Agreement Form

Name:

Date:

Course Name and Section Number:

I, the undersigned student, have read the safety information, pages 6-10, understood them and
agree to abide by the safety guidelines. I understand the importance of proper protection
(such as eye protection and other personal protection equipment) in the laboratory at all times.
I have also been warned about using contact lenses and understand that I should not wear
them in the laboratory. If I fail to abide by the safety rules, I will not hold Bilkent University,
course instructor(s) and teaching assistant(s) responsible for any injuries that result.

Signature of the Student:

Date:

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Table of Contents
Aim.........................................................................................................................................6
Safety......................................................................................................................................6
Chemical waste disposal.........................................................................................................6
Responsibilities.......................................................................................................................7
Grading...................................................................................................................................7
Emergency Procedures................................................................................................................9
Safety Rules..............................................................................................................................10
Common Laboratory Procedures..............................................................................................15
1. Using the balance.......................................................................................................15
2. Handling Solids..........................................................................................................16
3. Handling Liquids........................................................................................................16
4. Titration......................................................................................................................16
5. Filtration.....................................................................................................................17
Experiment 1: Volumetric Measurements................................................................................20
Experiment 2: Alkali and Alkaline Earth Metals......................................................................33
Experiment 3: Copper Recycling..............................................................................................47
Experiments 4-6:Identification of Common Chemicals...........................................................60
Experiment 4: Properties of Common Chemicals................................................................63
Experiment 5:Designing Tests For Distinguishing Common Chemıcals.............................69
Experiment 6:Identification of Unknowns............................................................................75

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 Aim
The experiments described in this manual are complementary to the material covered in the
class and deal with general chemistry topics. The labs are intended to familiarize you with
properties of the elements, safe handling of chemicals, chemical waste disposal, and usage of
laboratory equipment and glass wares.

Safety
Running a lab in a safe way does not mean that no dangerous substances will be used. Almost
all chemicals pose health risks. Running a lab safely means that dangerous substances will be
handled properly. Safety issues for dangerous substances are explained at the beginning of the
instructions for each lab. Read these explanations carefully before coming to the lab. You can
find additional safety information easily in the internet searching for material safety data
sheets (MSDS) and the name of the substance. Safety instructions for the chemicals that are
used regularly throughout the semester will not be repeated every time. You are expected to
know and to remember what you learned in the previous labs. For reference, all safety
instructions are also summarized in the beginning of this manual.

Chemicals that are not discussed in the safety issue sections are not very hazardous and are
handled with the usual care: Never taste or swallow, do not inhale, avoid skin contact, and
wear goggles to protect your eyes.

All safety instruction must be followed meticulously by students, lab assistants, and lab
technicians. There are no unnecessary safety precautions in this manual. Under no
circumstances may any of the safety instruction be ignored.

Do not change, especially do not increase, the amounts. Exothermic reactions can get out of
control, if the amount of substance is increased. Do not perform experiments other than the
ones in the manual. Any kind of fooling around with chemicals will lead to immediate
dismissal from the lab. Depending on the severity of the misbehavior, you may not be
readmitted and may fail the course.

Using latex gloves is not generally encouraged as many chemicals damage or penetrate latex
gloves. In fact there are many kinds of safety gloves for various kinds of chemicals and it
requires experience and knowledge to select the appropriate gloves. Wearing latex gloves may
give you a feeling of being protected while you are not. If bare hands are coming in contact
with chemicals, washing with copious amounts of water is usually sufficient. Wearing
damaged gloves, washing off chemicals is much more difficult.

Chemical waste disposal

In general, chemical waste may not be poured into the sink or be discarded in garbage bins,
since cleaning staff members might be endangered. Only non-toxic chemicals that may be
part of food can be poured in the sink in small amounts and in diluted form. Pay attention to
the waste disposal instructions given with the experiments.

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 Responsibilities
Attendance of all lab sessions is compulsory.

Failing to attend any lab session will result in failing the course.

You have to wear appropriate clothing (see safety rules) for all labs. You will not be
admitted to the lab with open shoes, shorts or short skirts because legs and feet are not
protected.

Long hair must be secured and lab coats must be worn, eye protection should never be
removed or pushed up. If you do not comply with these rules, you may be dismissed
from the lab and fail the course.

You have to be on time for the labs.

Up to 15 min late arrival: You will not be allowed to write the quiz and your quiz grade will
be zero. If you arrive late for a third time, you will not be admitted to the lab and might fail
the course.30 min late arrival: You will not be admitted to the lab and you might fail the
course.

Lab Procedures

Before coming to the lab you need to read the reading assignments given in the manual for the
experiment and you must go through the description of the experiment. Before performing an
experiment, consider all steps and be aware of all products and side-products formed. You
must be aware of physical state, chemical properties, and relevant safety precautions for all
hazardous chemicals involved.

Answer the pre-lab questions in writing. The pre-lab assignments will be collected at the
beginning of each lab. A short quiz regarding your reading assignment will be given before
starting the lab work. During the experiment data will be recorded in the data sheets.
Laboratory reports will be written in the lab when the experiment is completed. The
laboratory reports and data sheets (signed by your assistant) will be collected at the end of
each lab and evaluated.

Grading
Your grades for experiment 1-3 and 6 will consist of
 Pre-lab (20%) –handed to the assistants at the beginning of each experiment.
 Quiz (20%)
 Data Sheet (10%) – Should be signed by your assistant
 Laboratory Report (50%) – Should be handed to the assistants at the end of each experiment.
Experiments 4/5
 Prelab (40%)
 Lab Report (60%)
Experiment 6
 Lab Report (100%)

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 Emergency Phone Numbers

Fire (Campus) 6666

Fire (Ankara) 110 or 3414160

Ambulance (Campus) 6666

Ambulance (Ankara) 112

HealthCenter Main Campus 1666 1304 1392

Police 155 or 3840606 3035555

Chemistry Department Chair 2089 or 2664946

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 Emergency Procedures

In case of an alarm signal

Evacuate immediately through either one of the two emergency exits. Collect at the lawn in
front of the chemistry building, so that we can determine whether all students are safe.

In case a student gets spilled with a dangerous substance

Get the injured person under the body shower.Quickly remove any clothing contaminated
with chemicals. Be careful not to contaminate the eyes. Douse with water. Wrap the injured
person. Call for help (Tel. 6666)

In case a student splashes a corrosive chemical into her/his eye

Irrigate with plenty of water for at least 15 minutes. Check for and remove contact lenses.

A person’s clothes are on fire

Douse the individual with water or roll the person on the floor to cut the oxygen contact with
the part on fire.

A person is overcome with smoke or fumes

Remove the person to uncontaminated air.

In case of a spill of chemicals on the hands of a student

Wash with copious amounts of water.

In case of a spill
Contact the assistants for the proper clean-up procedure.

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 Safety Rules
1. Approved safety goggles must be worn in the lab at all times. It is forbidden to wear
contact lenses since chemicals can condense on them.

2. Closed shoes have to be worn. Sandals, open-toed, and open-topped shoes are not
permitted. Your body and clothes have to be protected with a cotton lab coat.

3. To minimize fire hazards, long hair must be confined securely. Do not wear loose fitting
or billowing clothing. Apart from the apparatus, only notebooks may be on the benches.

4. Students must know the locations of safety exits, fire extinguishers, and safety showers.

5. If any chemical comes into contact with the eyes, immediately flush with lots of water.

6. If any substance is spilled on skin or clothing, it must be washed off immediately with
plenty of water. Clothes must be removed if necessary.

7. The test tubes should not be opened pointing toward people.

8. Do not taste the chemicals.

9. Use fume hood for the reactions that involve poisonous gases.

10. Perform only the assigned work, specified in the lab manual. .

11. Eating, drinking, and smoking are forbidden. No food or drink should be brought to the
lab.

12. Coats and book bags must be placed out of the aisles.

13. Every student is personally responsible for the cleanliness of her or his bench top.

14. Chemical waste must be disposed of according to the instructions.

15. All containers containing chemicals must be labeled correctly.

16. Any incidences that compromise safety must be reported to the course instructor
immediately.

17. If a lab personnel do not follow the safety procedures, the course instructor must be
informed immediately.
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18. Making phone calls is strictly forbidden in the laboratory.

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Glassware

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a) Erlenmeyer flasks hold solids or liquids that may release gases during a reaction or
that are likely to splatter if stirred or heated.

b) A funnel is used for filtration or to aid in the transfer liquid from one vessel to
another.

c) Graduated cylinders are used to measure volumes of liquids. The glass cylinder has
etched marks to indicate volumes, a pouring lip, and quite often, a plastic bumper to
prevent breakage.

d) Beakers hold solids or liquids that will not release gases when reacted or are unlikely
to splatter if stirred or heated.

e) Test tubes hold small volume of liquid (less than about 5 mL).

f) Burets are used for titration. A titration is a laboratory procedure for quantitative
analysis.

g) A thermometer is used to measure temperatures. It should always be stored in its

plastic case to help prevent breakage. Place the tip of the thermometer below the
surface of the solution, but do not allow the tip to touch the walls or the bottom of the
flask. Determine the temperature by reading the scale on the thermometer at eye level.
Read the temperature by using all certain digits and one uncertain digit. Certain digits
are determined from the calibration marks on the thermometer. The uncertain digit
(the last digit of the reading) is estimated. On most thermometers encountered in a
general chemistry lab, the tenths place is the uncertain digit.

h) A glass rod is used to manually stir solutions. It can also be used to transfer a single
drop of a solution.

i) A volumetric flask is used to measure very precisely one specific volume of liquid
(25, 50, 100 ml, 250, 500, 1000 mldepending on which flask you use). This flask is
used to prepare a solution of known concentration. A volumetric flask should not be
used to heat substances or store solutions, and you should avoid pipetting directly
from the volumetric flask.

j) A wash bottle has a spout that delivers a wash solution to a specific area. Distilled
water is the only liquid that should be used in a wash bottle.

k) A watch glass is used to hold a small amount of solid, such as the product of a
reaction.

l) A pipet (or pipette) measures and delivers exact volumes of liquids. A pipet bulb is
used with a pipet to draw solution into the pipet. Bringing the final receiver under the
pipet and with pipet tip touching the flask wall let the solution to drain out. Continue
to touch the flask wall for5 seconds after the pipet looks empty. The pipets are
calibrated “to deliver” the specified quantity of liquid rather “to contain” it. What this
really means is that you should never blow the last drops of them.

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12
 Common Laboratory Procedures

1. Using the balance

The laboratory balance is used to measure masses. When using a balance, the most important
parts are the balance pan and the digital display. Balances with high precision, 0.0001 g, have
a draft shield as shown in the picture. The balances you will be using in the first year lab, do
not require a draft shield since they weigh only with a precision of 0.01 g.

Check that the balance pan is clean and dry. NEVER WEIGH A SAMPLE DIRECTLY ON
THE BALANCE PAN!

Choose a weighing vessel that can be used in subsequent steps of the experiment. A beaker
may be appropriate for weighing liquids to be heated, and an Erlenmeyer flask may be
appropriate for weighing substances that will generate a gas in subsequent reactions. A
weighing paper can only be used for weighing solids. Sometimes when nothing is on the
balance pan, the mass display will show a non-zero reading. Taring is used to set the mass
display to zero. Once the balance has been tared, the mass of any object set on the balance pan
will be displayed on the digital readout. The two types of taring techniques commonly used
are automatic and manual taring. If more than the desired amount of material is weighed,
place the excess material in an appropriate waste container. Never return excess or unused
chemicals to their original containers!

Before leaving the balance, clean up the area. Use a brush to clean all solids from the
balance pan, and wipe up any liquids. Wear gloves while cleaning if a material may be

13
hazardous. Also clean the area around the balance. Dispose of any excess or unused chemicals
in an appropriate waste container.

2. Handling Solids
Use a clean spatula to transfer solid from bottles. NEVER USE A CONTAMINATED
SPATULA. Also, NEVER RETURN UNUSED SOLID TO THE REAGENT BOTTLE. To
avoid waste, never remove more solid from a bottle than is necessary.

3. Handling Liquids
When transferring liquids from a reagent bottle, always place the stopper upside down in
order to avoid contamination. Pour the liquid slowly to avoid spillage. You may find the use
of a glass rod helpful, as shown below in Fig. 2.

Fig. 2. Liquid transfer

4. Titration
In a titration two reagents are mixed, one with a known concentration and one with an
unknown concentration. There is some way to indicate when the two reagents have reacted
essentially completely, and at the end of the titration the unknown solution's concentration can
be calculated. Typically, one reagent is a solution and is added from a buret. This solution is
called the titrant. The solution from the buret is added to a flask that contains either a
measured volume of a solution or a weighed quantity of solid that has been dissolved. The
buret has graduations that are used to read the volume of titrant added to the flask. Rinse a
clean buret several times with 5 mL portions of the titrant (the solution that will be added to
the flask). Allow the titrant to drain through the buret stopcock so that the tip gets rinsed with

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titrant as well. Discard the rinse solution in a waste beaker. Clamp the buret into place, and
fill it with the titrant. Remove air bubbles from the tip of the buret and the stopcock by
draining several milliliters of titrant. Dispose of the drained titrant in a waste beaker. Make
sure the volume reading in the buret is at the 0.00 mL mark or below (the meniscus does not
need to be on the 0.00 mL mark to begin the titration). Record the volume reading on the
buret. Determine the volume by reading from the bottom of the meniscus at eye level (Fig. 3).
The use of a card with a dark strip on it might be helpful in sharpening the image of the
meniscus. You will find by experiment that if the top of the strip is positioned slightly below
the level of the liquid in the buret, the bottom of the meniscus will be very easy to see. All
certain digits and one uncertain digit should be recorded.

Fig. 3. Reading the meniscus

5. Filtration
Filtration is a technique used to separate a solid from a solution. The two main types of
filtration are gravity filtration and vacuum filtration. Gravity filtration is most useful when the
solid is to be discarded and the filtrate (the liquid that flows through the filter paper) kept.

Fig.4 A gravity filtration

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To do gravity filtration you will use filter paper and a funnel. You must first flute the paper in
order to accelerate the process. This is shown in Fig. 4.

Fig. 4. Fluting the filter paper

Vacuum filtration is often faster than gravity filtration and is most useful if the solid must be
kept or if a filtration must be done rapidly. A vacuum from an aspirator or a vacuum pump is
used to pull the liquid through a funnel containing a piece of filter paper, while the solid is left
on the paper.

Fig.5 Vacuum filtration apparatus

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17
 Experiment 1: Volumetric Measurements

Purpose
The purpose of this laboratory is to practice performing precise volumetric measurements, to
determine the number of significant figures in measurements, and to learn handling significant
figures properly in calculations.

Introduction

Please read Chapter 1 of your textbook (11th ed.) to prepare for this experiment.

Important decisions (economic, social, and medical) are based on results of measurements.
Just a couple of examples of the huge importance of measurements:

 40% of the EU directives involve measurements;

 It has been estimated that direct spending on measurements alone make up ca 80
billion EUR or 1% of the GDP in Europe

A very significant part of all measurements are chemical measurements (chemical analyses).
Yet, in spite of their importance, all too often measurement results are of unsatisfactory
quality (i.e, are wrong). (Taken fromhttp://www.msc-euromaster.eu)

It is very important in chemistry as well as in other fields of science, to make measurements

precisely and accurately. Never forget that the road to a successful experiment starts with a
right measurement. In this experiment, the importance of a right measurement will be
demonstrated as well as showing how to make an accurate volumetric measurement using
different glassware. Some key concepts related to this experiment will be explained here
briefly.

Precision: The precision of a set of measurements refers to how closely individual

measurements agree with one another. The precision is good (or high) if each of the
measurements in a set is close to the average of the set.

Accuracy: The accuracy of a set of measurements refers to how close the average of the set
comes to the true, or most probable, value. Measurements of a high precision are more likely
to be accurate than those of poor precision, but even highly precise measurements are
sometimes inaccurate. Accuracy and precision are visualized in the following figure.

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Significant Figures: The significant figures (also called significant digits) of a number are
those digits that carry meaning contributing to its precision. For example, look at the
following table:

Measurement
1 1.233
2 1.235
3 1.231
4 1.230
5 1.236
Average 1.233

Notice that the five measurements agree in the first three digits but differ at the fourth digit.
Thus, the fourth digit is uncertain. All the digits known with certainty (three in this case) plus
the first uncertain one are called ‘significant figures’ (or digits). The more significant figures
we have in a measurement, the more precise the measurement is. Check out Chapter 1 Section
1.4 of your text book for more examples and details!

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In some cases, small changes in a digit far from the decimal point lead to changes in figures
closer to it (e.g. adding 0.0001 to 0.9999). In such a case it is necessary to take the average of
all measurements and to calculate the difference between each individual value and the
average. This method shows that the values in all three data series below have the same
differences from the average and therefore the same number of significant figures, although
they appear to have different precision at first glance.

examples for
measuremen
t series:
1 value-mean 2 value-mean 3 value-mean
0.552 0.000 0.558 0.000 0.998 0,000
0.551 0.001 0.557 0.001 0.997 0,001
0.553 -0.001 0.559 -0.001 0.999 -0,001
0.555 -0.003 0.561 -0.003 1.001 -0,003
0.550 0.002 0.556 0.002 0.996 0,002
sum 2.761 2.791 4.991
mean 0.5522 0.5582 0.9982
correct value 0.552 0.558 0.998

Safety
Be careful while handling glassware.

Waste Disposal
Waste disposal is not necessary for this experiment.

Apparatus and Materials

 2 Beakers (one 50 mL, one 100 mL)
 Erlenmeyer flask, stopper
 Graduated Cylinder
 Pipette (25 ml)
 Electronic balance

Procedure
Determining the density of water to the correct number of significant figures using an
electronic balance and different devices to measure the volume.
There are four balances in our labs. Two are able to determine masses with a precision of
1/10000 of a gram, two only with a precision of 1/100 of a gram. Both kinds of balances can
be used for this experiment and all figures given by the balances should be recorded. As both
types of balances are more precise than the devices used for the volumetric measurements, the
precision of your measurements is limited by the precision with which you can determine the
volume. Your task is to determine the precision of your volume measurements.

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In this week’s experiment water is used, which does not pose any health hazards. Take this
opportunity to practice clean working. Pretend you are handling a strong acid. Do not lose one
drop, do not spill any water on the bench, and do not get any water on your hands or clothes.

a) Volumetric measurements with a beaker

 Fill the 100 mL beaker with tap water and use it as a reservoir. Now transfer 20
mL to the 50 mL beaker. Fill it as accurately as possible to the 20-mL mark. You
have to check the reading with your eye at the same level as the water-air
interface.

 Take the beakers and the Erlenmeyer flask with the stopper to one of the electronic
balances. If the balance does not show 0.0000g, tare the balance by pressing the
button “T”. Now determine the mass of the empty Erlenmeyer flask with the
stopper and write it down.

 Take the Erlenmeyer flask off the balance, place it on the bench and transfer the 20
ml of water from the measuring beaker to the Erlenmeyer flask. Do not fill the
Erlenmeyer when standing on the balance! Close it with the stopper. If the flask
is not closed, evaporation of water will make weighing on precision balances
impossible, as the weight will keep decreasing.

 Weigh the stoppered Erlenmeyer flask with the water and record the weight in the
table below.

 Pour the water back to your reservoir beaker.

 Carry out the procedure five times. Make sure your equipment is dry on the
outside. There is no need to dry the inside of the Erlenmeyer, if you determine the
‘empty’ weight of the wet Erlenmeyer before each weighing.

 Determine how many significant figures your measurements have by comparing

the five values. Underline the significant figures of each measurement.

b) Volumetric measurements with a graduated cylinder

 Fill the graduated cylinder as accurately as you can to the 20-mL mark. The
cylinder is gauged so that the bottom of the meniscus has to be at the 20-mL mark.

 Take your cylinder, reservoir beaker, and Erlenmeyer flask with stopper to the
electronic balance.

 Weigh the empty Erlenmeyer flask.

 Pour the 20 mL of water into the Erlenmeyer flask, stopper it and weigh it. Do this
five times, just as in step a).

 Record your measurements in the table. Determine the number of significant

figures.

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c) Volumetric measurements with a pipette
 Take a pipette and pipette ball to transfer 20 mL of water. Be careful with the
pipettes. These are expensive precision instruments.
 Take the reservoir beaker with the water, the pipette and the Erlenmeyer flask with
stopper to the bench next to the balances.
 Determine the mass of the ‘empty’(wet) flask. Place the rubber ball on the pipette.
This has to be done gently. Otherwise, the glass may break. Use slight twisting
motions, if the ball does not move easily. Do not insert the glass too far, since it
has to come off easily.
 Now squeeze the ball a little bit. Insert the tip of the pipette into the water and suck
in the water by pressing on point “S” or “↑”. Take more than 20 mL but do not
suck water into the ball.
 Lift the pipette out of the water and dry it with paper on the outside. Do not touch
the opening and suck water on the paper. Make sure no air bubbles get in.
 Adjust the water to exactly 20.00 mL by using point E or “↓”.
 Now transfer the water to the Erlenmeyer flask. Tilt the flask and touch the tip of
the pipette to the glass of the flask. Let the pipette run out slowly (it should take
about 30-60 s). Wait five more seconds, drain the pipette one more time touching
the wall of the flask. Do not try to remove the remainder of the water that remains
inside the tip of the pipette. Pipettes are gauged accounting for this remainder. No
water droplets should remain on the walls of the pipette. Otherwise your
measurement is wrong and must be repeated.
 Stopper the Erlenmeyer flask and weigh it.
 Repeat the procedure five times and record the results.

For all measurements calculate the density and round to the correct number of significant
figures in the last column of the table. Compare precision and accuracy of the
measurements with the three devices. Try to remember this experiment and always obey
the rules for handling significant figures in your homework and exams.

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Name: Section:

Experiment 1 Pre-lab Questions

1. Describe precision and accuracy and the relation between these two concepts.

2. Determine how many figures in the following data set are significant and enter the
numbers with correct number of significant figures in the last column of the table.

Measurements Acquired data Correct significant figures

1 1.2457
2 1.2458
3 1.2407
4 1.2453
5 1.2425

3. Draw the following glassware: Beaker, Pipette, Erlenmeyer flask, Graduated Cylinder,
Watchglass, Test tube, and Volumetric flask.

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24
Name:

Exp. 1 Data Sheet

Density
Beaker Empty Mass Total Mass Mass of water Density
correct s.f.
Measurement1
Measurement2
Measurement3
Measurement4
Measurement5

Graduated Density
Empty Mass Total Mass Mass of water Density
cylinder correct s.f.
Measurement1
Measurement2
Measurement3
Measurement4
Measurement5

Density
Pipette Empty Mass Total Mass Mass of water Density
correct s.f.
Measurement1
Measurement2
Measurement3
Measurement4
Measurement5

Assistant’s Signature:

_________________

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Name: Section: Date:

ID number:

Partner(s):

Experiment 1: Laboratory Report

Purpose

Observations

Conclusion
How do the devicesyou used for the volumetric measurements compare interms of their
accuracy and precision? Use this section of the lab report to express any other thoughts that
you may have for this experiment.

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Discussions
1. What kind of glassware should one use to make an accurate volumetric measurement
of any given liquid? Give two examples of accurate glassware used in the laboratory.

2. Perform the following calculation and round off the answer to the correct number of
significant figures.

49.146 m + 72.13 m – 9.1434 m = ?

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 Experiment 2: Alkali and Alkaline Earth Metals

Purpose
The purpose of this laboratory practice is to observe the most prominent properties of alkali
and alkaline earth materials. The experiments in this section will include reactions of alkali
and alkaline earth metals with water, flame color tests and solubility tests for alkali and
alkaline earth metals.

Introduction
Read Chapter 21, Group 1 and 2 elements in your textbook (11 th ed.) to prepare for this
laboratory.

The alkali metals are a series of chemical elements in the periodic table. This group gets its
name from the fact that all its metal hydroxides are strongly basic. In the modern IUPAC
nomenclature, the alkali metals are called the Group 1 elements. The group 1A metals
exhibit regular trends for a number of properties. As we would expect, radii of the alkali metal
atoms and ions increase regularly from Li to Cs because the number of electron shells
increases in proceeding down the group. There is also a regular decrease in the first ionization
energies as you go down since larger atoms can be stripped of their ns 1 electron more easily
compared to smaller atoms. The decrease in electronegativity from top to bottom is also
related to the increase in size and shows the increase in metallic character.

The alkali metals have two notable physical properties; softness and low melting points. All
are soft enough to be scratched with a toothpick and cut with a knife. The melting points of
cesium and rubidium are low enough to make both of them liquid on a very hot day. Alkali
metals react directly with water, producing hydrogen gas. The reactivity of the alkali metals
increases in higher rows of the periodic table. For this experiment reactivity of Li and Na will
be demonstrated and compared.

Alkaline earth metals are Group 2 elements according to the periodic table. Early chemists
gave the name "earths" because they are less soluble in water than alkali metals. As a result,
alkaline earth metals are usually found in the continental crust, while alkali metals tend to
concentrate in the oceans. The main minerals in which magnesium is found are carnellite,
magnesite, and dolomite. Calcium is found in chalk, limestone, gypsum, and anhydrite.
Magnesium is the eighth most abundant element in the Earth’s crust, and calcium is the fifth.

The metals of Group 2 are harder and denser than sodium and potassium, and have higher
melting points. These properties are due largely to the presence of two valence electrons on
each atom, which leads to stronger metallic bonding than in Group 1.

Group 2 shows the same general trends of increasing atomic radii and decreasing ionization
energies from top to bottom as group 1. The higher densities of group 2 metals in comparison
to group 1 metals are mainly a consequence of the large difference in atomic sizes between

28
the two groups. Molar volumes are significantly smaller in group 2 than group 1 and the
molar masses are only slightly larger.

Safety
Lithium (Li) and sodium (Na)
 Flammable, corrosive, react violently with water, strong acids, and chlorinated
solvents
 Fires cannot be extinguished with water or carbon dioxide. Dry sand can be used.
 Cause skin burns. In case of contact wash with copious amounts of water.

Magnesium metal (Mg)

 Flammable, burns with a flame so bright that it can damage the eyes
 Reacts with water producing a flammable gas (H2)

Hydrochloric acid (HCl(aq))

 Causes burns and irritates the respiratory system
 In case of skin contact, wash with water.

Sodium fluoride (NaF)

 Toxic, liberates a poisonous gas (HF) upon contact with acids

Nitrates
 Oxidizing materials, contact with combustible substances may cause fire.

Barium chloride (BaCl2) and all other barium compounds

 Toxic upon ingestion.

Strontium chloride (SrCl2) and all other strontium compounds

 Toxic upon ingestion.

Waste Disposal
Because the amounts are so small, and the gathering procedure mixes acid with base, disposal
at the sink with very large amounts of water is appropriate. Discard the wet paper towels with
ordinary solid trash.

Apparatus and Materials

 Porcelain bowl
 Spatula
 Concentrated hydrochloric acid
 Watch glass
 Test tubes
 Wires for flame tests

29
Using the Bunsen Burner
The burner consists of a metal tube attached to a stand, a turning knob to adjust the gas flow,
and a metal ring to adjust the air flow. The gas is supplied by a rubber tube that is connected
to wall outlet. The wall outlet has a yellow lever that stops the gas flow when it is in the
perpendicular (closed) position. Make sure that the gas is turned off completely when the
burner is not in use.

To light the burner, proceed as follows:

 Make sure that the yellow level is in the perpendicular position.

 Place the burner on the desk so that you can work conveniently. It should not be too
far back so that the shelves do not catch fire and not too far to the front, so that you do
not get burned. Make sure that you can reach the yellow lever without leaning over
the burner.

 Close the air supply holes on the bottom of the burner by turning the metal ring until
the holes are covered.

 Turn the screw of turning knob on the burner clockwise as far as possible to reduce
the gas flow to a minimum. Be aware that this knob only regulates the gas flow but
does not stop it completely.

 Now have one hand on the yellow lever (without leaning over the burner) and ignite
the lighter with the other hand. Hold the lighter over the Burner and move the yellow
lever towards the parallel (open) position until the gas above the burner ignites.

30
  If the gas does not ignite, close the gas and the lighter and wait a moment. This way
gas does not collect on the desk and ignite all of a sudden. Then repeat the procedure.

 When the burner ignites, there will be a small yellow flame. The flame size can be
increased by adjusting the turning knob on the burner. The yellow flame is not used to
heat anything because it produces a lot of soot and is not very hot. The yellow flame
is useful when the burner is not used for a short time but will be needed again.

 For using the burner, the combustion of the gas must be made more efficient by
letting air flow through the air hole on the bottom. First increase the flame with the
turning knob and then slowly open the air holes until a blue cone appears. Now the
burner is ready for use.

 The zone directly above the inner blue cone is the hottest part of the flame and reach
1000 ºC.

 The inner part of the blue cone is the reducing zone because there is little oxygen
available.

 The outer zone of the flame is the oxidation zone because air oxygen is available to
oxidize the heated sample.

 Never leave the burner unattended with a blue flame because it can be hard to see and
you or others might get burned. Simply close the air holes and reduce the gas flow to
produce a bright orange flame.

 Always be careful to avoid burns and never heat a material too quickly or explosive
“bumping” can occur. Control the heat transfer by adjusting the distance from the
burner to the object.

Materials
The following chemicals: Lithium metal (Li(s)), sodium metal (Na(s)), magnesium metal
(Mg(s)), lithium chloride (LiCl), lithium carbonate (Li 2CO3), sodium fluoride (NaF),

31
 sodium chloride (NaCl), sodium carbonate (Na 2CO3), sodium nitrate (NaNO3), sodium
sulfate (Na2SO4), sodium phosphate (Na3PO4), potassium chloride (KCl), potassium
carbonate (K2CO3), potassium sulfate (K2SO4), potassium nitrate (KNO3), magnesium
nitrate hexahydrate (Mg(NO3)2·6 H2O), magnesium chloride hexahydrate (MgCl 2·6 H2O),
magnesium sulfate heptahydrate (MgSO4·7 H2O), calcium nitrate tetrahydrate
(Ca(NO3)2·4 H2O), calcium sulfate (CaSO4), calcium carbonate (CaCO3), calcium
hydroxide (Ca(OH)2), strontium chloride hexahydrate (SrCl2·6 H2O), strontium nitrate
(Sr(NO3)2), barium chloride dihydrate (BaCl2·2 H2O), and barium nitrate (Ba(NO3)2)

Procedure
1. Perform all the steps of this experiment in the fume hood behind the protective
glass. Fill a porcelain bowl with water. Cut a small piece of Li and put it in the water
carefully. Record your observations. Next use sodium. Take a small piece, about pea-
size. Do not use more sodium or an explosion might occur. Liquid sodium might
splash around! Do not touch sodium with your fingers.

Waste: The water phase in the bowl is strongly basic and must be collected in the
waste container for bases.

2. Fill a test tube with cold water and add some Mg filings. Observe for a while.
Compare with the behavior of Li and Na. Add a few drops of phenolphthalein. Does
Mg react with cold water?

Waste: The solution is basic and should be collected in the container for bases.

3. In a small beaker, prepare a solution of NaF. Keep it as a reagent.

4. Collect small amounts (the tip of small spatula) of the chemicals listed above in dry
test tubes. Do not take more substance or the following experiment will be
inconclusive. Try to take about the same amount of each substance. At your work
place, look at the tubes, notice differences in appearance of these chemicals and take
notes. These notes will be useful for labs4-6.

Do the following steps 5-8 for all of your substances:

5. Add deionized water to the test tube containing one of the substances until the test
tube is filled to no more than one fifth of its volume (about two fingers high). Swirl
the tube with circular motions of your wrist and observe whether the substance
dissolves completely in cold water. If it dissolves, the mixtures become clear and
transparent. Make sure to record whether dissolution is fast or slow. If the mixture
looks cloudy and opaque, dissolution is incomplete. Give it some more time. If the
mixture remains cloudy apply heat by holding the test tube with the lower end into the
flame of a Bunsen burner. Point the opening away from yourself and other people,
swirl slightly and heat carefully to avoid splashing. Observe whether the substance
dissolves in hot water. Keep the solution for the following experiments. If it still
appears cloudy after heating, let the solid settle and decant the clear liquid into a fresh
test tube. Record your observations in the table below.
32
6. Take a platinum wire for the flame tests and hold it into a Bunsen burner flame. Make
sure that there is no color, otherwise the wire needs to be cleaned with water, rinsed
with deionized water, and glowed until no color appears. Using the solution from step
4, carefully dip the clean wire in the solution and then remove. There should be a
small amount of solution retained on the loop at the end of the wire. Place the wire
loop in the hottest part of the Bunsen burner flame and observe and record any color
change in the flame. The colors of some substances disappear fast. Repeat the test
until you are sure of your observation.
7. Check and record the pH value of the solution from step 5with universal indicator
paper.
8. Try whether a precipitate forms if sodium fluoride (NaF) solution is added to the
solution from step 4. If a precipitate forms, write a net ionic equation.

Waste:

Barium and strontium compounds have to be discarded in the containers labeled

‘heavy metals’.

Fluoride solutions have to be collected in a container.

Small amounts of the other salt solutions can be poured into the sink and flushed down
with water.

33
Name: Section:

Experiment 2 Pre-lab Questions

1. In which order does the reactivity of alkali metals increase? Explain its reason.

2. Why do alkali elements not occur in pure form in nature?

3. Why do alkali and some alkaline earth metals produce flame colors? Explain briefly.

4. How does the solubility change between 2nd and 6th rows of the periodic table for
alkali and alkaline earth metals salts? Does the anion in a salt affect its solubility?

34
Name:

Exp.2Data Sheet

Task 1: Note your observations.

Task 2: Note your observations.

35
Tasks 4-7:

Compound soluble in Soluble Flame Color pH of Reaction with

cold water with solution NaF
heating
LiCl

Li2CO3

NaCl

Na2CO3

NaNO3

Na2SO4

Na3PO4

KCl

K2CO3

KNO3

K2SO4
MgCl2·2
H2O
Mg(NO3)2·6
H2O
MgSO4·7
H2O
Ca(NO3)2·4
H2O
CaSO4

CaCO3

Ca(OH)2

SrCl2·6 H2O

Sr(NO3)2
BaCl2·2
H2O
Ba(NO3)2

Assistant’s Signature:_________________

36
Name: Section: Date:

ID number:

Partner(s):

Experiment 2: Laboratory Report

Purpose

Observations

Chemical reaction(s)
Write the chemical reactions for experiments 1&2:

37
Discussions
1. How do the reactivities of alkali and alkaline earth metals for their reactions with
water compare?

2. Do anions affect the flame color of alkali and alkaline earth metals in their different
compounds? How do the solubilities of alkali and alkaline earth metals compare.
Which anions tend to form insoluble compounds?

38
 3. Why do some of the dissolved salts form a precipitate when NaF is added to the
solution? Explain.

Conclusion
Do you think flame colors can be used as a reliable method for the characterization of alkali
and alkaline earth metals? Do you see a trend for the solubility of alkali and alkaline earth
metals in the periodic table? Use this section of the lab report to express any other thoughts
that your may have on this experiment.

39
 Experiment 3: Copper Recycling
Introduction
This experiment provides a means of becoming acquainted with some techniques of working
carefully with metals in acid. The goal is to dissolve a copper disk in acid and, through a
series of reactions, recover the copper. A scheme of the entire series of reactions follows,
where the symbols over the arrows indicate concisely the reagents or techniques used in each
step.

Copper dissolves in either concentrated nitric acid (equations (1, 2 and 3)) or in dilute nitric
acid (equations (4, 5 and 6)). Each of these chemical reactions can be described by three
chemical equations: a molecular equation, a full ionic equation and a net ionic equation. The
molecular equation gives the formula of the reactants that are added together and treats all
products as if they exist as intact compounds.

Copper dissolving in concentrated nitric acid

Cu(s) + 4 HNO3(aq) →Cu(NO3)2(aq) + 2 NO2(g) + 2 H2O (1)

The molecular equation can be used to write the full ionic equation in which all aqueous
strong electrolytes (strong acids, strong bases, and soluble ionic compounds) are broken into
their respective aqueous ions.

Cu(s) + 4 H+(aq) + 4 NO3¯(aq) → Cu2+(aq) + 2 NO3¯(aq) + 2 NO2(g) + 2 H2O (2)

For any substance that appears on both sides of the chemical equation, an equal number of
moles of that substance can be removed from the chemical equation. In the full ionic equation
there are four moles of nitrate on the reactant side of the equation and two moles on the
product side. Therefore, two moles of nitrate can be removed from both sides of the equation
to yield that net ionic equation.

Cu(s) + 4 H+(aq) + 2 NO3¯(aq) → Cu2+(aq) + 2 NO2(g) + 2 H2O (3)

Copper dissolving in dilute nitric acid

Molecular equation

3 Cu(s) + 8 HNO3(aq) → 3 Cu(NO3)2(aq) + 2 NO(g) + 4 H2O (4)

Full ionic equation

3 Cu(s) + 8 H+(aq) + 8 NO3¯(aq) →3 Cu2+(aq) + 6 NO3¯(aq) + 2 NO(g) + 4 H2O(5)

40
Net ionic equation

3 Cu(s) + 8 H+(aq) + 2 NO3¯(aq) →3 Cu2+(aq) + 2 NO(g) + 4 H2O (6)

The two reactions can be distinguished from one another since NO 2(g) has a red-brown color
and NO(g) is colorless. Two equilibria confuse the issue, however, as represented by
equations (7) and (8).

2 NO(g) + O2(g) →2 NO2(g) Keq = 2.32 x 1012 (7)

2 NO2(g) ⇌N2O4(g) Keq =6.86 (8)

N2O4(g) is also colorless. Because of these complications, most reactions of nitric acid with
copper look similar. The reaction with concentrated nitric acid is much more rapid, however,
and it is this one that we shall use.

Note: NO2(g) is a deadly poison! To quote from a reliable source*: “One of the most
insidious gases. Inflammation of lungs may cause only slight pain or pass unnoticed, but
the resulting edema several days later may cause death. 100 ppm is dangerous for even a
short exposure, and 200 ppm is fatal.”In a laboratory of average size, 100 ppm = 18.6 g =
0.404 mol = the amount of NO 2 produced by dissolving 12.8 g Cu, or approximately four
copper disks. It is therefore essential that you work in the hood when dissolving the disk in
nitric acid. This warning is included so that you can protect yourself if some NO 2 is released
in the laboratory. If you notice NO2 fumes outside the hood, do not stand around. Leave
the laboratory immediately!

*Martha Windholtz, ed., The Merck Index, 10th ed., Gahway, NJ: Merck and Co., 1983, p.
947.

We would find it very difficult to recover the copper from this strongly oxidizing acidic
nitrate solution, since any elemental copper produced will be oxidized immediately by the
excess nitrate ion present according to equations (4) through (6). This oxidation of copper
metal is catalyzed by the presence of acid. Accordingly, we shall remove as much as possible
both the H+ and NO3¯ from the solution.

Addition of sodium hydroxide solution to the blue acidic copper(II) nitrate solution causes
two things to happen. First, the hydrogen ion in solution reacts with the added hydroxide ion
to form water. The hydrogen ion is effectively removed from the solution.

H+(aq) + OH¯ (aq) → H2O

Second, the copper(II) ion forms an insoluble substance with the hydroxide ion, copper(II)
hydroxide. The copper(II) hydroxide produced is difficult to work with since it is a rather
gelatinous white precipitate (with some traces of blue). Therefore, we heat the solution to
produce black copper(II) oxide.

41
This still leaves the nitrate ion in solution, but this is removed by decanting the liquid. You
want to allow the black copper(II) oxide to settle to the bottom and then carefully pour out the
supernatant solution—the solution on top of or above a solid—making sure not to lose any of
the solid. Some nitrate ion will still be present, so we add some hot water, stir, allow the
copper(II) oxide to settle, and then decant the liquid again. This process is called “washing”
the precipitate— in this case the copper(II) oxide. Since you will need about 150 mL of
almost boiling water to do this, you can save considerable time if you put the water on to boil
at the beginning of the laboratory period.

The copper is now on the bottom of the beaker in the form of copper(II) oxide, and we would
like to have it in solution. This is done readily by adding sulfuric acid. The copper(II) oxide,
which is basic, reacts with sulfuric acid to produce a copper(II) sulfate solution with a striking
blue color.

Since sulfuric acid will not dissolve copper (try it with a piece of copper wire if you are
skeptical), we can now recover the copper from the solution by reducing it with zinc. This is
accomplished by adding fine particles of zinc to the solution. Of course, zinc also reacts with
the excess acid to produce hydrogen, so large quantities of gas are evolved on the addition of
zinc. Be careful that the hydrogen produced is not released into the laboratory because it can
explode. This reaction must be performed under the hood. The excess zinc is removed by
adding some hydrochloric acid.

The only solid now left is copper, which must be dried so that it can be weighed. If you do
this over a Bunsen burner flame, the copper will react with the oxygen in the air to produce
black copper(II) oxide. Consequently, wash the copper first with methanol to remove the
water and then with acetone, which will rapidly evaporate. The acetone is removed by
evaporation over a hot plate or over a steam bath (Figure 2).

Safety Precautions

Review the safety rules on pages 5 and 8-9 of this manual.

Work in the hood when dissolving the copper disk with nitric acid, and when adding granular
zinc or hydrochloric acid to the mixture.

Keep methanol and acetone away from all open flames. Both substances are extremely
flammable.

Add all reagents slowly, because rapid addition may cause an unexpectedly fast reaction that
may spatter.

Stir the copper hydroxide solution constantly while it is being heated to prevent spattering.

Use insulated gloves, or beaker tongs (not crucible tongs), to handle vessels containing hot
water or hot solutions, but be careful that the vessel does not slip out of the gloves or tongs
and break.Practice first with a 400 mL beaker filled with cold water.

42
Use graduated cylinders to measure the liquids (pipets and volumetric flasks are not required).

Procedure (George F. Condike, J. Chem. Educ., 52, 1975, p. 615.)

1. Working in a group of four weigh a piece of copper (about 1.5 g) to the nearest
milligram. Place it in a 400 mL beaker.

2. Place 150 mL of distilled water in a 250 mL beaker. Place the beaker on a wire gauze
on a ring stand, and heat with a bunsen burner until the water boils. Do not wait for
the water to boil but proceed with the rest of the experiment. You will use this hot
water in step 6.

3. In the hood add 12.0 mL (use a graduated cylinder) of concentrated nitric acid to the
copper disk in the beaker. When the reaction is complete (the copper disk is gone and
no gas bubbles are being produced) add 25 mL of water. You may now take the
beaker out of the hood. Be careful. The beaker may be hot! When the beaker has
cooled so that it may be handled safely, pour its contents into a 100 mL graduated
cylinder. Rinse the beaker with two 2.5mL portions of distilled water and add this to
the graduated cylinder. Add distilled water to bring the total volume to 50 mL.
Carefully stir the solution with a glass stirring rod to assure that the solution is
homogeneous. Measure 25.0 mL of solution into 100 mL beakers for each group (of
two students), rinsing the graduated cylinder with distilled water into the last beaker.
The remainder of the experiment will be done in groups of two using the 25 mL of
solution. This solution corresponds to one half of the copper.

4. Prepare 45 mL of 3.0 M NaOH. Calculate how much solid NaOH you need and show
the result to your assistant before you proceed. Be careful when making the solution
as the reaction is exothermic and the mixture gets quite hot. Add the 45mL of 3.0 M
sodium hydroxide solution to form copper(II) hydroxide. Stir well. Observe the color
changes.

5. Add two or three boiling chips. Then, with gentle stirring, heat the solution just to
boiling to convert the copper(II) hydroxide to copper(II) oxide. Do not stir violently
because the copper(II) oxide will not settle in the next step when it is too finely
dispersed. Be very careful to heat gradually and just until the black copper(1I) oxide
is formed from the blue-white copper(II) hydroxide. Too much heat will cause the
solution to bump and spatter all over you. If you do not add the boiling chips, your
solution will “bump” when you heat it and spatter out of the beaker. The boiling
chips prevent this by giving the vapor bubbles a place to form. Place the beaker on
the bench top. Use beaker tongs (not crucible tongs) or insulated gloves to move the
hot beaker.

6. Allow the solid to settle and then decant the supernatant liquid into another beaker.To
decant means to carefully pour off the liquid making sure that none of the solid goes
with it. Decant, do not use plastic pipets!Using a glass rod as shown on page 14 will
help. It is sufficient to let the solid settle for 2 to 3 min or until about a 2 cm depth of
43
 relatively clear liquid appears at the top of the mixture. Add about one-third (50mL)
of the very hot water you prepared, stir up the solid for about 15 sec, allow the solid
to settle, and decant the hot water. Repeat this with two more portions of very hot
water. Handle the beakers with insulated gloves or beaker tongs. Thorough washing
is important to remove the soluble sodium and nitrate ions as completely as possible.

DISPOSAL
Decanted solutions: Add phenolphthalein and, if basic, neutralize with 6 M H 2SO4
(first disappearance of pink color). Flush this salt solution down the sink with running
water.

7. Prepare 25 mL of 6.0 M H2SO4. Calculate how much H2SO4(conc) (18 M) you need
and show the result to your assistant before you proceed. Be careful when making the
solution as the reaction is exothermic and the mixture gets quite hot. Make sure to
add the acid slowly to the water and not reverse. If you pour water in the concentrated
acid, hot acid might splash all over you. Add the25 mL of 6.0 M H2SO4 solution to
produce copper(II) sulfate. Stir this mixture to get it to react completely. It will also
get somewhat warm and you would be wise to hold the beaker with tongs or insulated
gloves. Make sure that all the black copper(ll) oxide dissolves. You may have to
scrape some of this black solid down from the top edges of the beaker with a wet
stirring rod. Decant the solution into another beaker and discard the boiling chips.

8. In the hood, add 3.0 g of 30-mesh zinc metal slowly to precipitate copper metal. Stop
adding if the reaction foams a lot. Wait until the foaming stops, then resume adding
zinc. Stir until the supernatant solution has become colorless. If the reaction ceases
and the solution remains blue, add a small additional amount of zinc. Be careful
towards the end to not add excessive amounts of zinc or it will take a long time to
destroy the extra zinc. When no blue color is present and you can no longer observe
gas being formed, decant the supernatant liquid into another beaker. Discard the
liquid once you are sure no solid has been transferred.

DISPOSAL
Acid-zinc(II) solution: Mix and save for combining with waste from step 11.

9. Still in the hood, add 10.0 mL of distilled water and then 15.0 mL of concentrated
hydrochloric acid to destroy the excess zinc. When the evolution of gas bubbles has
become very slow, warm, but do not boil, the mixture. Do not warm the mixture too
much. A maximum temperature of about 60°C is what you are trying to attain.

10. While you are waiting for the gas to stop evolving, weigh a porcelain evaporating
dish to the nearest mg. When you can no longer see any gas bubbles forming, add 50
ml of distilled water, remove from the hood, and stir. Then decant and discard the
supernatant liquid into another beaker. Repeat washing with 50 mL of water, decant
the washing water and transfer all the solid (use a glass rod) to the weighed
evaporating dish. You may use some distilled water to help in transferring the solid.

44
 DISPOSAL
Acid-zinc(II) solution: Mix and save for combining with waste from step 11.

11. Add 10.0 mL total of distilled water to the solid, stir the mixture to make sure that all
the solid is washed, and decant the distilled water into a beaker. Repeat this washing
with two more 10.0 mL portions of distilled water. Discard the decanted distilled
water.

DISPOSAL
Acid-zinc(II) solution: Combine with the waste solutions from steps 8 and 10. Add
phenolphthalein and neutralize with 6 M NaOH (first appearance of pink color).
Dispose in a waste bottle labeled heavy metals solutions.

12. Wash the solid with 10 mL of methanol. (This substance is highly flammable. Keep it
away from flames !) Decant the liquid into a beaker, and discard the washings.

DISPOSAL
Methanol/acetone:Dispose in a waste bottle labeled organic—aliphatic—
nonhalogenated or labeled with the compound names.

13. Wash the solid with 10 mL of acetone. (This substance is highly flammable. Keep it
away from flames !) Decant the liquid into a beaker, and discard the washings.

DISPOSAL
Methanol/acetone: Follow instructions for disposal in step 12.

14. Evaporate the remaining acetone by placing the evaporating dish on a hot plate or on
a steam bath as illustrated in Figure 28- 1 . Ensure that the evaporation is as complete
as possible by stirring the solid with a glass rod. When dry, the fine particles of
copper metal will be granular and will no longer adhere to the stirring rod.

15. Dry as much of the evaporating dish as you can (don’t forget the bottom). You can
use
the paper towels to dry the evaporating dish. Do not get overzealous and try to dry the
copper, for some of it will stick to the paper towels and be lost. Wait for the
evaporating dish to cool and weigh it with your product to the nearest milligram.

16. If you have enough time, repeat steps 14 and 15 until two successive weights are the
same. Good chemists always perform this final step to make sure that their product is
completely dry.

DISPOSAL
Copper metal: Put in a recycling bottle labeled copper metal.

45
Figure 1. Two Methods for Evaporating Off Acetone

46
Name: Section:

Experiment 3 Pre-lab Questions

1. What is the safety precaution associated with dissolving a copper disk?

2. What are the name and chemical formula of the product of the reaction in step 4 of the
procedure?

3. What are the name and chemical formula of the gaseous product of the reaction in step 8 of
the procedure?

4.What are the name and chemical formula of the solid product of the reaction in step 8 of the
procedure?

5. What is meant by the phrase “washing the precipitate”?

47
48
49
Partner(s): Section:

Experiment 3: Laboratory Report

1. (a) Write the full balanced molecular equation and the balanced net ionic equation for the
reaction that has occurred in each of the following steps. Indicate the state of matter of
each species in the balanced equations. (b) Classify the reaction by type (combination,
decomposition, single displacement, metathesis, or redox). Note that more than one
classification type may fit— for example, a reaction may be single displacement and
redox. If so, indicate both types. (c) State what leads you to conclude that a reaction has
occurred (evolution of a gas, change of color, heat, light, sound, formation of a
precipitate, or any combination).

Step 3

Molecular equation ___________________________________________________________

Net ionic equation___________________________________________________________

Classification ___________________________________________________________

Observations ___________________________________________________________

Step 4

Molecular equation ___________________________________________________________

Net ionic equation ___________________________________________________________

Classification ___________________________________________________________

Observations ___________________________________________________________

Step 5

Molecular equation ___________________________________________________________

Net ionic equation ___________________________________________________________

Classification ___________________________________________________________

Observations ___________________________________________________________

50
Partner(s): Section:

Experiment 3: Laboratory Report

Step 7
Molecular equation ___________________________________________________________

Net ionic equation ___________________________________________________________

Classification ___________________________________________________________

Observations ___________________________________________________________

Step 8 (two reactions)

Molecular equation ___________________________________________________________

Net ionic equation ___________________________________________________________

Classification ___________________________________________________________

Observations ___________________________________________________________

Molecular equation ___________________________________________________________

Net ionic equation ___________________________________________________________

Classification ___________________________________________________________

Observations ___________________________________________________________

Step 9
Molecular equation ___________________________________________________________

Net ionic equation ___________________________________________________________

Classification ___________________________________________________________

Observations ___________________________________________________________

51
2. Was your percent recovery of copper greater than or less than 100%? Describe an
experimental error that could have caused this. What could be done to prevent this error?

52
 Experiments 4-6:Identification of Common Chemicals
________________________________________________________________

Introduction

The main purpose of this and the following two experiments is to familiarize yourself with
some of the properties of common chemicals. In addition, you will gain experience with
several physical and chemical methods that are commonly used in chemical analysis. Finally,
by developing your own scheme for identifying the various chemicals, you will begin to learn
how to plan an analysis logically and will gain some appreciation for the method of scientific
investigation.

Your objective for this experiment is to develop a series of tests that will allow you to identify
the chemicals listed in Table 1. You must find properties for each chemical that allow you to
distinguish it from all of the others in that table. This experiment is divided into three parts. In
Part A, an assortment of chemicals and methods of identification are examined. Part B
focuses on distinguishing the chemicals from the others. Part C is a test to be taken by all
students in the last lab session of this course.

If you keep careful records of your results in your laboratory notebook, you will be able to
devise a complete scheme for the identification of any of the chemicals as soon as you have
tested the last of them. Then you only need to try out your scheme to see that it works well.

Safety Precautions

Review the safety rules on pages 5 and 8-9 of this manual.

Wear goggles at all times.

Never taste any chemical.

Smell chemicals by fanning some of the vapors toward your nose and then only when
specifically directed to do so by your instructor. Never smell a reaction mixture when it is
being heated or when it is reacting.

If you must touch chemicals or if you inadvertently get chemicals on you, wash immediately
with soap and large volumes of running water. Report any contact with chemicals to your
instructor.

Use small quantities of chemicals as directed. Compare the amounts you take with those in
labeled test tubes prepared by your instructor or weigh the chemicals.

Stay at a distance from a reaction mixture while it is being heated.

Never use anything but a glass stirring rod to mix chemicals. If you can, mix chemicals by
gently tapping the side of a test tube with your finger. (Have your instructor demonstrate this

53
technique.)

Never bring large quantities of liquid near an open flame.

Dispense reagents either with the dropper or spatula supplied with each bottle or by pouring
out a small quantity of liquid or solid reagent. No more than 0.5 mL (10 drops) of liquid or
0.3 grams (size of 3 grains of rice) of solid should be taken back to your bench for testing.
Chemicals should be dispensed into your smallest sized test tubes, not into flasks or beakers.

Do not return excess reagent to a bottle; it may contaminate the rest of the contents. Instead,
throw it away in the manner and place designated by your instructor, normally in the
appropriate waste container.

DISPOSAL

Unreacted metals: Rinse and recycle in a bottle labeled for that metal.
Solids: (1) NaCl, NH4Cl, CaCl2, CaO, SiO2, NaHCO3, CaCO3, K2CO3, CaSO4, borax, and
sucrose may be disposed directly into the room trash container. (2) All other solids should be
disposed in a waste bottle labeled common chemica1s—so1id wastes.

Solid solution mixtures: Filter into a waste bottle labeled common chemicals-aqueous
wastes. The solids will be put into the solid waste bottle.

Aqueous solutions: Solutions of the salts listed in solids (1) above, acetic acid, acetone,
alcohols, and ethylene glycol may be rinsed down the sink with running water. Other aqueous
solutions must be put in a waste bottle labeled common chemicals—aqueous wastes.

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Table 1. Study Set of Common Chemicals
___________________________________________________________________________

Mg magnesium metal
Al aluminum metal
Zn zinc metal
C carbon, solid
S sulfur, solid
MnO2 manganese(IV) oxide, manganese dioxide
KMnO4 potassium permanganate
LiCl lithium chloride
Li2CO3 lithium chloride
NaCl sodium chloride
NH4Cl ammonium chloride
CaCl2 calcium chloride
SrCl2 strontium chloride
Cu(NO3)2•3H2O copper(ll) nitrate trihydrate, cupric nitrate trihydrate
Ni(NO3)2•6H2O nickel(ll) nitrate hexahydrate
NaHCO3 sodium bicarbonate, sodium hydrogen carbonate
Li2CO3 lithium carbonate
CaCO3 calcium carbonate
K2CO3 potassium carbonate
FeS iron(II) sulfide, ferrous sulfide
KAl(SO4)2•12H2O alum, aluminum potassium sulfate dodecahydrate
CaSO4 calcium sulfate
CuSO4•5H2O copper(II) sulfate pentahydrate
Na2SO3 sodium sulfite
Na2B4O7•10H2O borax, sodium tetraborate decahydrate
K2CrO4 potassium chromate
CrCl3 chromium(III)chloride
Cr2O3 chromium(III)oxide
Cr(NO3)3 chromium(III)nitrate
C12H22O11 sucrose, table sugar
HNO3 3 M solution of nitric acid
HCl 6 M solution of hydrochloric acid
H2SO4 6 M solution of sulfuric acid
HC2H3O2 6 M solution of acetic acid
NaCl 3 M solution of sodium chloride
NH3(aq) 6 M solution of ammonia
NaOH 6 M solution of sodium hydroxide
CH3OH wood alcohol, methyl alcohol, methanol
C2H5OH grain alcohol, ethyl alcohol, ethanol
(CH3)2CO acetone
C6H12 cyclohexane

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 C2H4(OH)2 ethylene glycol, 1,2-ethanediol

Experiment 4: Properties of Common Chemicals

___________________________________________________________________________

Procedure

1 . On the reagent shelf you will find labeled bottles of the different chemicals listed in Table
1. Your task is to devise a series of tests that will enable you to distinguish between the
various chemicals.
2. Some tests will be quite simple, such as looking at a substance and observing its color and
texture. You may smell the chemicals if you have your instructor’s explicit permission to
do so. But, do so cautiously by opening the bottle and fanning some of the vapors toward
your nose. Do not taste the chemicals! Since many chemicals are similar in appearance,
you would do well to devise a confirming test.
3. All the chemical tests should be performed with a drop of liquid or a piece of solid no
larger than a match head. Larger quantities will waste chemicals, yield ambiguous results,
and may produce dangerous reactions.
4. You should begin by looking up the physical and chemical properties of the substances;
use your textbook, the internet, or the library. Two good reference books are the
Handbook of Chemistry and Physics and The Merck Index.You may also use the results of
your laboratory work throughout the semester.
5. Some of the tests that you might wish to use follow. Try these tests in the order listed until
you find a test that gives definite results.
a. Rate of evaporation.
b. Viscosity. How readily does a liquid flow?
c. Solubility. Make sure that the solid is finely divided and try to dissolve an amount of
solid the size of a match head in 0.5 mL of water.
d. Color of a dilute aqueous solution.
e. Effect of aqueous solutions or pure liquids on litmus paper. Acidic solutions turn blue
litmus red. Basic solutions turn red litmus blue.
f. Reaction with precipitating agents, such as BaCl 2(aq) and AgNO3(aq). Test 1 drop of
your aqueous solution on a spot plate with 1 drop of precipitating agent.
g. Solubility in solvents other than water, such as ethanol.
h. Ability to decolorize a dilute solution of KMnO4 (reducing power).
i. Reactions with a strong (NaOH) and a weak [NH3(aq)] base.
j Reactions with a strong (HCl) and a weak (HC2H3O2) acid.

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 k. Flammability and/or color of the flame. Test one drop of the liquid or the aqueous
solution held on a loop of nichrome wire.

6. Precautions
a. Some of the chemicals are highly poisonous. Do not taste any of the chemicals.
b. Many of the liquids are highly flammable. Do not bring large quantities of any
liquid near an open flame.

7. After you have made your observations, carefully plan your tests for the next lab. Record
all information in your notebook. You will only be allowed the use of your notebook
during the testing period in the final lab.

Name: Section:

Experiment 4 Pre-lab Questions

1 . What is the first step in identifying a chemical?

2. How is a solid substance dissolved in water?

3. How is a flame test performed?

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4. How is litmus paper used in identifying a chemical?

5.When is it permissible to taste a chemical?

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Partner(s): Section:

Experiment 4: Laboratory Report

Describe the experiments you performed and briefly comment on the results, include
ambiguous outcomes, difficulties to distinguish substances, and so on.

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60
 Experiment 5:Designing Tests For Distinguishing Common Chemıcals
___________________________________________________________________________

Try out your tests by having another student select several chemicals for you to identify.
Modify your tests if necessary.
Some Suggestions for Tests

Your investigation of the common chemicals is best done in a systematic fashion. Indeed, part
of the purpose of these laboratories is to develop your skill in designing and carrying out an
experiment. You should keep in mind that in Part B you will have only a limited amount of
time to test each chemical and therefore, your procedures should be as simple as possible.
There are two consequences of this: First, you do not want to perform more tests than are
absolutely necessary. Thus, you should ask yourself the question: Does this last test uniquely
identify this chemical? Discard any tests that don’t contribute more knowledge about the
chemical. Second, since physical tests (color, liquid or solid, viscosity, etc.) are generally
easier and faster than chemical tests, it is to your advantage to devise as many physical tests
as you can.

Specific Suggestions

1. Start simply. Note everything that you can about a substance before you open the bottle,
including answers to the following questions.
a. Is it a solid or a liquid?
b. What is its color?
c. If it is a liquid, does it flow easily? That is, is it viscous or not?
d. If it is a solid, is it shiny or dull? How large are the particles?

2. Open the bottle and take out a match head sized piece of solid or 5drops of liquid. Here
again you can make a number of observations.
a. What does it smell like? Do this with caution by waving some of the vapors toward
your nose, not by snorting the vapors directly over the bottle. Some of the smells
(ammonia and acetic acid, for example) are so characteristic that you can stop here.
Do not forget to smell the solids also. But do not smell anything unless specifically
directed to do so by your instructor.
b. If it is a liquid, does it have a high (a drop beads up on a glass plate) or a low (a drop
spreads out) surface tension?
c. If it is a liquid, is it volatile (the drop evaporates rapidly) or nonvolatile? High surface
tension and low volatility usually go together.
d. If it is a solid, does it crush easily? (What is its tensile strength?) Try to crush it with
the end of a glass rod. Does it look different when it is crushed?

3. Try dissolving about 0.1 g of the crushed solid in 0.5mL of distilled water in a small test
tube using a stirring rod to agitate the mixture.
a. Does it dissolve easily?

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 b. What is the dolor of the solution?
c. Did any gas evolve, did you hear anything, or was any heat produced when you
dissolved it in water? In other words, did a chemical reaction occur with water?
d. Does the freshly prepared solution have a smell? Get your instructor’s permission
before you smell a solution.

4. Test the solution or the liquid sample chemically. Chemical reactions are best done using
one drop of reagent on a spot plate.
a. Is it acidic, basic, or neutral? Dip the stirring rod into the solution and touch it to a
piece of litmus paper. Using this method, one piece of litmus paper can be used to test
several solutions. If itturns blue litmus red, the solution is acidic; if it turns red litmus
blue, the solution is basic. If no change occurs in either case, the solution is neutral.
b. Add a drop of possible precipitating agent to one drop of liquid sample on a glass plate
and see if a precipitate appears. Possible agents are dilute H 2SO4, dilute NaOH, dilute
HCl, dilute AgNO3, and dilute BaCl2.
(1) Did a precipitate appear? What color is it?
(2) Did a reaction occur and perhaps change the color of the solution (what is the new
color?) or produce a gas (what does the gas smell like?)? (Before you smell the gas,
get your instructor’s permission.)
c. Add a drop of dilute KMnO4 solution (light purple) to 3 drops of the solution. Does
the KMnO4 turn colorless?’ Is any gas evolved? What is the new color of the
solution?
d. Try a flame test. Put a drop of solution on a loop of wire and carefully evaporate the
liquid in the coolest part of the Bunsen flame. Repeat this twice. You now have a
concentrated solution or some solid on the wire loop. Place this in the hottest part of
the Bunsen flame and observe the brief flash of co1or. It is difficult to perform
correctly without practice. (Many people incorrectly substitute a chunk of solid for the
drops of solution. This shortcut often gives a misleading color to the flame and also
tends to ruin the Bunsen burner when the melted solid drops down inside.)
5. Only if the solid does not dissolve in water, try to dissolve it in another solvent. First
(HCl, HNO3, H2SO4) and bases (NH3, NaOH) and then concentrated acids and bases if
necessary. All tests that you can perform on the aqueous solution (see 3 and 4 above)
are valid on the solution produced at this point.
6. In summary, if you are careful, you can avoid several errors. Always work with small
quantities of chemicals. Too much material is not only wasteful but also produces poor
results. Practice the tests a couple of times and make sure you get the same results
each time. Make sure that you have have at least two positive tests for each
identification. Don’t distinguish between two substances on the basis of only one test,
especially if the results are difficult to interpret.

62
Name: Section:

Experiment 5 Pre-lab Questions

Write a plan for disinguishing the chemicals that are similar at first sight, e.g. white solids,
colorless liquids, and so on. You will work according to your own plan during this lab.

Any copied pre-labs will lead to dismiss form this lab and failure of the
course!

63
Name: Section:

Experiment 5 Lab Report

Describe the tests you performed, describe your observations, and analyze possible problems
when the tests are used for proving the presence or the absence of a chemical.

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65
 Experiment 6:Identification of Unknowns
___________________________________________________________________________

A selection of 16 chemicals from those studied will be placed in numbered bottles. The test
will be given during this last laboratory period. You will be permitted the use of only your
laboratory notebook during the test.

Example: A Scheme to Identify Five White Solids

A student isto find tests that distinguish among five white solids: Ba(NO 3)2, BaCl2, KNO3,
NH4NO3, C7H6O2 (benzoic acid). Any useful test must allow the substances being tested to be
divided into atleast two groups based on the results of the test. Therefore, color and state of
matter are not useful properties since all the compounds are white solids.

ProposedProcedure:

1. Test the solubility in water. Result: All are quite soluble, except benzoic acid; therefore,
benzoic acid is distinguished from the others.
2. Of the remaining four solids, three are nitrate salts and one is a chloride salt. Therefore, a
test to distinguish chloride from nitrate is appropriate. Recall from the solubility rules that
Ag+ ions form a precipitate when mixed with Cl¯ ions. A small amount of each solid is
dissolved in 5 drops of water. One drop of AgNO3is added to one drop of each of the four
solutions. Result: A white precipitate of AgClis observed in the solution of BaCl2.
3. The three remaining solids all have nitrate as the anion. Therefore, they must be
distinguished based the properties of the cation. Recall from the solubility rules that
BaSO4 is insoluble. One drop H2SO4 is added to one drop of each of the three solutions.
Result: A white precipitate of BaSO4is observed in the Ba(NO3)2 solution.
4. Solutions of the two remaining solids can be tested for acidity using litmus paper. Result:
NH4NO3 is acidic and KNO3 is neutral.
5. The flow chart inFigure 1 summarizes the procedure used to identify the five solids. It
can serve as a quick reference during a test.

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Figure 1. Flow Chart of Proposed Procedure

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68
Name: Section: ID:

Lab Report Experiment 6: Identification of Unknowns

Please write the name of the compound& provide a brief explanation about how you
determined each ion or compound. Explain each step concisely.

Compound #1:



Compound #2:


Compound #3:



Compound #4:

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Compound #5:



Compound #6:



Compound #7:



Compound #8:



Compound #9:



Compound #10:


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71