SEFAKO MAKGATHO HEALTH SCIENCES UNIVERSITY

SCHOOL OF SCIENCE AND TECHNOLOGY

DEPARTMENT OF CHEMISTRY AND CHEMICAL SCIENCES

_.,,.-.-
. 1.x,-, - !
r--- ,_A ---..._,·..--,

SEFAKO MAKGATHO
H:EALTH SCIENCES UNIVERSITY

GENERAL CHAMISTRY lA
(MCHM0ll)

PRACTICAL MANUAL

2025 ACADEMIC YEAR

 EXPERIMENT 1: IDENTIFICATION OF COMPOUND PHYSICAL PROPERTIES

OBJECTIVES:

To identify a substance on the basis of its physical properties. To learn how to properly
assemble melting point and/or boiling point apparatus

INTRODUCTION:

Gold is yellow, table salt is white and crystalline, lead is "heavy,• and water is a colourless,
clear liquid that melts at 0°C and boils at 100°C. These are physical- properties of
substances that are often used for identification. The more common physical properties
include colour, odour, density, solubility, melting point, boiling point, and state of the
substance (solid, liquid, or gas). Physical properties can be observed or measured without
any knowledge of the chemical reactivity of the substance. Additional tests, tests that
reveal more information about its chemical or physical properties, may be necessary to
confirm the purity of the substance. The purpose of this experiment is to identify a
substance from the data collected on its solubility, density, melting point and/or boiling
point.

SOLUBILITY:

The solubility of a substance is the maximum mass (usually in grams) that dissolves in a
fixed mass (usually 100 g) of solvent at a given temperature. A substance has different
solubilities in different solvents, reflecting the differences in the molecular compositions of
the substance and the solvent. For instance, some substances, such as table salt, are
soluble in water but insoluble in gasoline. In this experiment we examine the solubility of a
substance in three different solvents: water (H2O), ethanol ( HsOH), and acetone,
(CH3)2C0. If further solubility tests are required, cyclohexane, (Ct.H12), will be used as a
solvent. QuaHtatively each substance is recorded as being soluble (complete dissolution)
or insoluble. Two liquids are immiscible when they are insoluble in one another.

DENSITY:

Each pure substance exhibits its own set of intensive properties. One such property is the
density, the mass of substance per unit volume. In SI system, the density of water at 4°c
is 1.00g/cm3• By measuring the mass and volume of a substance, its density can be
calculated. In this experiment, the densities of a water-insoluble metal and an unknown
liquid are detennined. The data for the mass arid the volume of water displaced are used
to calculate the density of the water-insoluble metal. A substance with a high density has a
large mass in a small volume. We commonly say that lead is "heavy." What we really
mean is that lead has a high density; the volume of lead need not be large to have a large
mass.

MELTING POINT:

A solid that is slowly heated changes completely to a liquid phase at a specific temperature
called the melting point. At the melting point, the solid and liquid phases coexist; any
lowering of the temperature results in the formation of only solid a • g of the
temperature results in the existence of only the liquid phase.

3
BOILING POINT:

When a liquid is gradually heated, there is a temperature at which bubbles form

spontaneously. These continue to form until the entire volume of the liquid has been
converted to a gas. This constant temperature is called the boiling point of the liquid, a
temperature at which the liquid and vapor phases coexist. The boiling point of a liquid
depends on the prevailing atmospheric pressure. (Boiling point: the temperature at which
the vapor pressure of a liquid equals the atmospheric pressure). (The atmospheric
pressure: the force that a column of air exerts over an area of the Earth's surface). The
melting and boiling points of a substance are characteristic of the magnitude of the forces
acting between molecules, called intermolecular forces. The greater the magnitude of
the intermolecular forces (i.e., the stronger the attraction between molecules), the higher
the melting and boiling points of the substance. As the magnitude of the intermolecular
forces is different for each substance, each has a characteristic melting point and boiling
point. (Intermolecular forces: interactive attractions and repulsions between molecules).

EXPERIMENTAL PROCEDURE:

A. Solubility

1. Solubility in Water: To a 75-mm test tube add a small amount (about the size of
the head of a match stick) of given solid or 3 drops of the given unknown liquid
to 1 ml of water. Swirl or agitate the contents. Does your unknown dissolve?
Record your observations.

2. Solubility in Ethanol and Acetone. Repeat the test with ethanol and acetone as
solvents. (Caution: Avoid the inhalation of vapors; acetone is flammable! Keep
away from flames). Describe the solubility of your unknown as soluble or
insoluble in each solvent.

3. Solubility in Cyclohexane. Additional solubility tests can be conducted using

cyclohexane as a solvent.

B. Density of Unknown Liquid

Complete two trials to determine the density of given unknown liquid.

1. Determine Mass and Volume. Determine the mass (±0.01 g) of your smallest
laboratory beaker. Pipette 2 ml of the liquid into the beaker and measure the
combined mass. (Note: use a rubber pipette bulb in drawing the liquid into the
pipette.) Calculate the density of the liquid.

C. Melting Point of Unknown Solid

With the help of a demonstrator, assemble the melting point apparatus using a
360gC thermometer. Note that the oil is the liquid that is heated. Complete two
measurements for the melting point of your unknown.

1. Prepare the Sample. Fill a capillary melting point tube to a depth of 0.5 cm with
the unknown solid. Compact the solid to the bottom of the tube. Attach the tube
to a 360gC thermometer with a rubber band (or band of rubber tubing). Place
the sample alongside the thermometer bulb.

4
 2. Determine the Melting Point. Slowly heat the oil bath at a rate of 5°C per
minute until the solid melts. (Caution: the oil bath may be at a temperature
greater than 100°c, do not touch!) Cool the oil bath until the sample solidifies;
at a rate of 1•c per minute, heat the bath until the solid again melts. Cycle the
cooling and heating of bath until the melting point of the solid has been
accurately determined. Disposal: Dispose of the capillary tube in the "Solid
Wastes" container. After the oil has cooled to room temperature, return it to the
"Used Oil" container.

D. Boiling Point of Liquid Unknown

With the help of a demonstrator, assemble the boiling point apparatus using a
110°C thermometer. Complete two measurements for the boiling point of unknown
compound.

1. Assemble the Boiling Point Apparatus. Place 10 drops of the unknown liquid
into a 75-mm test tube. (Caution: The liquid may be flammable, keep it away
from an open Bunsen flame!) Position it beside the thermometer bulb using a
rubber band. Invert (open end down) a 10-cm capillary melting point tube in the
liquid. Place the apparatus into the water bath.

2. Measure the Boiling Point. Place 2-3 boiling stones in the water bath. Slowly
heat the water in the water bath while stirring with the stirring rod. When a
rapid and continuous stream of bubbles escapes the capillary tube, discontinue
heating the water bath. The stream of bubbles slows as the bath cools. When
the bubbles cease to escape and before the liquid re-enters the capillary tube,
record the temperature. This is the boiling point of the liquid.

3. Repeat the Measurement. Determine the boiling point a second time. The
same (volume of) liquid may be used; however, the capillary tube must be
removed, emptied, and inserted before heating resumes. Disposal: Dispose
of the leftover unknown substance in the "Waste Organics" container.

PRE-LABORATORY ASSIGNMENT

Identification of a Compound: Physical Properties

1. From your general experiences, would you select water or petrol to try dissolving the
following? Explain.

a. table sugar (sucrose)

b. table salt (sodium chloride)
c. cooking oil (Crisco oil)
d. coal tar
e. blood serum

2. Define:

a. solubility
b. melting point
c. boiling point
d. density

5
3. Task

A student's unknown liquid boils at approximately 69°C, and is insoluble in water, but
soluble in ethanol. Its measured density is 0.65 g/mL. Use your textbook and/or
Library resources to identify the unknown substance.

4. Using the method described above when should the boiling point of a liquid be
recorded?

REPORT SHEET

EXPERIMENT 1: TABLE OF RESULTS - PHYSICAL PROPERTIES

A. SOLUBILITY OF SAMPLE NO: SOLUBLE INSOLUBLE

1. SOLVENT WATER

2. SOLVENT ETHANOL

3. SOLVENT ACETONE

B. DENSITY OF LIQUID SAMPLE NO: TRIAL 1 TRIAL 2

1. MASS OF TEST TUBE + BEAKER+ LIQUID (G)

2. MASS OF TEST TUBE + BEAKER (G)

3. MASS OF LIQUID (G)

4. VOLUME OF LIQUID (CM3)

5. DENSITY OF LIQUID (G/CM3)

6. AVERAGE DENSITY OF LIQUID (G/CM3)

C. MELTING POINT OF SOLID SAMPLE NO:

OBSERVED MELTING POINT

AVERAGE MELTING POINT

D. BOILING POINT OF LIQUID SAMPLE NO:

OBSERVED MELTING POINT

AVERAGE MELTING POINT
NAME OF UNKNOWN:

LABORATORY QUESTIONS:

I. How does atmospheric pressure affect the boiling point of a liquid? Ask.your lecturer.
2. If several drops of unknown liquid {Part B) cling to the pipette wall after delivery, will
the density of the unknown liquid be reported too high or too low? Explain.
3a. In Part D.2, suppose the boiling point is recorded when bubbles are rapidly escaping
the capillary tube. Will the boiling point of the liquid be recorded too high or too low?
Explain.
b. If the boiling point is recorded when the liquid enters the capillary tube (after the heat
is removed), will it be recorded too high or too low? Explain.

6
EXPERIMENT 2: IDENTIFICATION OF COMPOUND CHEMICAL PROPERTIES

OBJECTIVES:

To identify a compound in solution on the basis of its chemical properties. To design a

systematic procedure for analyzing a solution for the presence of a particular compound
Introduction: In this experiment, you will observe chemical reactions that are characteristic
of various chemicals under laboratory conditions. After collecting and organizing your data,
you will be given a chemical that you have previously investigated. The interpretations of
your collected data will assist you in identifying the chemical. What observations will you
be looking for? One or more of the following generally accompanies chemical changes: A
gas is evolved. This evolution may be quite rapid or it may be a "fizzing" sound. A
precipitate appears (or disappears). The nature of the precipitate is important; it may be
crystalline, it may have colour, it may merely cloud the solution. Heat may be evolved or
absorbed. The reaction vessel becomes warm if the reaction is exothermic or cools if the
reaction is endothermic. A color change occurs. A substance added to the system may
cause a color change. The chemical properties of the following compounds, dissolved in
water, are investigated in Part A of this experiment:

Sodium chloride NaCl (aq)

Sodium carbonate Na2C03 (aq)
Sodium sulphate MgSO4 (aq)
Ammonium chloride NH4CI (aq)
Water H20 (I)

(Chemical property: characteristic of a substance that is dependent on its chemical

environment). The following test reagents are used to identify and characterize these
compounds:

Silver nitrate AgNO3 (aq)

Sodium hydroxide Noah (aq)
Hydrochloric acid HCI (aq)

In Part B of this experiment the chemical properties of five compounds in aqueous

solutions, labeled 1 through 5 are investigated. For this investigation, three reagents
labelled A, B, and C will be used. From your observations, you will be required to devise
an analysis scheme that leads to the identification of an unknown in the least number of
steps.

EXPERIMENTAL PROCEDURE:

Procedure Overview: A series of tests for the chemical properties of known compounds
are conducted. A similar series of tests are conducted on an unknown set of compounds.
In each case, an unknown is identified on the basis of the chemical properties observed.
To organise your work, you will conduct a test on each known solution (there are five) and
the unknown solution with a single test reagent It is therefore extremely important that you
are organised and that you, as best possible, note down your observations. The Report
Sheet included shows a possible summarized "reaction matrix" for your observations.

7
A. Chemical Properties of Known Compounds:

1. Observations with Silver Nitrate Test Reagent. Set up a clean set of test tubes.
Place 5-10 drops of the five "known" solutions in test tubes A1-A5. Use a
dropper pipette (or a dropper bottle) for the delivery of the silver nitrate
solution. (Caution: AgN03 forms black stains on the skin. The stain, caused by
silver metal, causes no harm.) If after adding about five drops you observe a
chemical change, add 5-10 drops to see if there are additional changes.
Record your observations in the reaction matrix on the Report Sheet.

2. Observations with Sodium Hydroxide Test Reagent. Place 5-10 drops of the
five "known" solutions in Test tubes 81-85. To each of these solutions slowly
add 5-10 drops of the sodium hydroxide solution; record any observations
made as you add the solution. Check to see if a gas evolved in any of the
tests. Check for odors. What is the nature of any precipitates that form?
Observe carefully.

3. Observations with Hydrochloric Acid Test Reagent. Repeat Part A.1 in Test
tubes C1-C5; use the hydrochloric acid test reagent for the solutions and
record your observations. Check to see if any gas is evolved. Check for odor.
Observe carefully.

4. Data Analysis for Unknown. On the basis of the data you have collected and
summarized in the reaction matrix, devise a procedure by which you can
identify the compound in your unknown solution with the fewest number of
tests. Disposal: Discard the test solutions in the 'Waste Salts" container.
CLEANUP: Rinse the test tubes twice with tap water and once with distilled
water. Discard each rinse in the "Waste Salts" container.

B. Chemical Properties of Unknown Compounds

1. Preparation of Solutions. On the reagent shelf are five solutions, labelled 1

through 5, each containing a different compound. Use the test tubes as your
testing laboratory. The test tubes should be less than half full (about 1 ml) with
the test solutions.

2. Application of the Reagents. Use a dropper pipette (or a dropper bottle) to

deliver Reagents A through C to the solutions. If, after adding several drops,
you observe a chemical change, add 10-15 drops to see if there are additional
changes.

3. Testing the Solutions. Test each of the five solutions with 3-5 drops (and then
excess drops) of Reagent A Observe carefully and describe any evidence of
chemical change; record your observations. With a fresh set of
solutions, test each with Reagent B. Repeat with Reagent C.

4. Organization of Data. An unknown will be issued that is one of the five

solutions. Devise a scheme by which the unknown can be determined with the
least number of steps in the analysis. Disposal: Discard the test solutions in
the 'Waste Salts" container. CLEANUP: Rinse the test tubes twice with tap
water and once with deionized water. Discard each rinse in the "Waste Salts"
container.

8
PRE-LABORATORY ASSIGNMENT

Identification of a Compound: Chemical Properties

1. Refer to your textbook/lecture and determine which of the following salts are
considered insoluble(Give their correct scientific names).

a. NaN03
b. Mg(OH)i
c. NH4N03
d. MgCb
e. Ag2C03
f. AgCI

2. Three test tubes, with no labels, are in a test tube rack on the laboratory bench.
Lying beside the test tubes are three labels: potassium iodide(KI), silver
nitrate(AgN03), and sodium sulfide(Na2S). You are to place the labels on the test
tubes using only the three solutions present. Here is your test:

A portion of Test Tube 1 added to a portion of Test Tube 3 produces a yellow, silver iodide
precipitate.

A portion of Test Tube 2 added to a portion of Test Tube 3 produces a black, silver sulfide
precipitate.

How do you label your test tubes:

Test Tube 1 _
Test Tube 2 _
Test Tube 3 _

REPORT SHEET

IDENTIFICATION OF A COMPOUND: CHEMICAL PROPERTIES

A. Chemical Properties of Known Compounds

Unknown Sample Number:

Test NaCl(aq) Na2C03(aq) MgSO4(aq) NH4Cl(aq) H2')(1)

AgN03(aq)

NaOH (aq)

HCl(aq)

The compound in the unknown solution is:

9
B. Chemical Properties of Unknown Compounds

Test 1 2 3 4 5
A
B
C

The compound in the unknown solution is:

LABORATORY QUESTIONS

1. Three test tubes, with no labels, are in a test tube rack on the laboratory bench.
·Lying beside the test tubes are three labels: silver nitrate (AgNO3), hydrochloric acid
(HCI), and sodium carbonate (Na2CO3). You are to place the labels on the test tubes
using only the three solutions present. Here is your analysis procedure:

A portion of Test Tube 1 added to a portion of Test Tube 2 produces carbon dioxide
gas,

A portion of Test Tube 1 added to a portion of Test Tube 3 produces a white, silver
carbonate precipitate. On the basis of your observations how would you label the
three test tubes? What would you expect to happen if a portion of Test Tube 2 is
added to a portion of Test Tube 3?

2. Use the data from Experiment 3, Part A to predict what may be observed from a
mixture of:

potassium carbonate and hydrochloric;

acid zinc chloride and silver nitrate;
magnesium chloride and sodium hydroxide ;
ammonium nitrate and sodium hydroxide .

In an "unknown" solution only one of the following cations is present: Ag+, Ba2+,Mg2+,
or cu2•. The following experimental data were collected.

NH3(aq) HCl(aq) H2S04(aq)

Ag+ No change White ppt 0
No change
Ba2+ No change No change White ppt
Mg2+ White ppt No change No change
Cu2+ Blue ppV No change No change

Deep blue solution with excess. (Example: When an aqueous solution of

hydrochloric acid is added to a solution containing Ag+, a white precipitate (ppt)
forms.). Write the formula of the insoluble silver salt. Write the formula of the
insoluble barium salt.

10
EXPERIMENT 3 : CHEMISTRY OF. COPPER

OBJECTIVES

To observe a number of chemical changes of copper in a series of reactions. To use

several techniques to recover copper from solution.

INTRODUCTION

In previous laboratory experiments we were able to take advantage of the physical and
chemical properties of a substance for identification. In this experiment, we take that
understanding one step further. Copper is an element that is chemically found combined
into a variety of compounds in nature, most commonly in the form of a sulphide, as in
chalcocite, Cu2S, and chalcopyrite, FeCuS2. Copper metal is an excellent conductor of
heat and electricity and is an alloying element in bronze and brass. Capper is a soft metal
with a characteristic bright orange-brawn colour, which we often call "copper colour".
Copper is relatively inert chemically; it does not readily oxidize in air (react with oxygen in
air) and is not attacked by simple inorganic acids such as sulphuric and hydrochloric acids.
Copper(ll) ion forms a number of very colorful compounds; most often, these compounds
are blue or blue-green, although other colors are found depending on the copper(II)
compound. We will observe many of the chemical and physical properties of copper by
cycling copper through a series of reactions that produce a number of colorful compounds.
Dissolution of Copper Metal. Copper reacts readily with substances called oxidizing
agents (substances that remove electrons from other substances). In this experimen1
aqueous nitric acid, HNO3, is the substance that oxidizes or copper metal, Cu(0), to
copper(II) ion.

Cu(s) + 4HNOa(aq) Cu (NO3h(aq) + 2NO2 (g) + 2H2O (I)

In this reaction copper (!!)nitrate, Cu(NO3)z, is a water-soluble salt that produces a blue
solution, and nitrogen dioxide, NO2, is a dense, red-brown gas. The solution remains acidic
because an excess of nitric acid is used for the reaction. Precipitation of Copper(II) ion
from solution. The solution containing the soluble Cu(NO3)2 is made basic with sodium
hydroxide, NaOH. Copper(II) hydroxide, Cu(OHh, a light blue compound, precipitates
from the solution.

Cu(N03)2(aq) + 2 NaOH(aq) Cu(OH)2(s) + 2 NaNOJ(aq)

Sodium nitrate, NaNO3, is a colorless salt that remains dissolved in solution.

Conversion of Copper(ll)hydroxide to a second insoluble salt. Heat applied to the

copper(II) hydroxide causes black, insoluble copper(II) oxide, CuO, to form.

Cu(OH)2(s) ) CuO(s) + H2O(I)

Dissolution of Copper(ll)oxide. Copper(ll) oxide dissolves readily in aqueous sulphuric

acid, H2SO4, to form a sky blue solution due to the formation of the water-soluble salt,
copper{II) sulfate, CuSO4.

11
Re-formation of Copper Metal. The addition of magnesium metal, Mg, to the copper (II)
sulphate solution completes the copper cycle. In this reaction, magnesium is a reducing
agent (a substance that provides electrons to another substance). Magnesium reduces
copper (II) ion, Cu2+,in the copper (II) sulphate solution to metallic copper and water-
soluble magnesium sulphate, MgSO4.

CuSO4 (aq) + Mg(s) Cu(s) + MgSO4 (aq)

Magnesium metal also reacts with sulphuric acid. Therefore when magnesium metal is
added to the copper(II) sulphate solution, a second reaction occurs that produces
hydrogen gas, H2, and additional magnesium sulphate.

Therefore, hydrogen gas bubbles are observed during the reaction. This reaction is also
used, to remove any excess magnesium metal that remains after the copper has been
recovered.

EXPERIMENTAL PROCEDURE

Procedure Overview: Copper metal is successively treated with nitric acid, sodium
hydroxide, heat, sulphuric acid, and magnesium to reproduce the copper metal. The
chemical properties of copper are observed in the cycle.

A. Metallic Copper to Copper(II) Nitrate

Preparation of the Copper Metal Sample. Obtain a less than 0.02g sample of Cu
wool from your laboratory instructor. Determine the mass (±0.001 g) of a 75-mm test
tube. Roll and place the Cu wool into the test tube and measure their combined
mass. Reaction of the Copper Metal. Perform this step in the fume hood. Using a
dropper bottle or a dropper pipette, add drops (< 10 drops) of concentrated HNO3
until no further evidence of a chemical reaction is observed. (Caution: concentrated
HNO3 is very corrosive, do not allow it to touch your skin. If it does, wash
immediately with excess water. Nitric acid will tum your skin yellow). At this point the
Cu metal has completely reacted. (Caution: do not inhale the evolved nitrogen
dioxide gas). What is the colour of the gas? Add 10 drops of distilled water. Show the
resulting solution to your laboratory instructor for approval and save the solution for
Part B.

B. Copper(II) Nitrate to Copper(II) Hydroxide

1. Preparation of Copper(II) Hydroxide. Agitate or continuously stir with a stirring

rod the solution from Part A.2 while slowly adding 1O drops of 6M NaOH.
(Caution: Wash immediately with water if the NaOH comes into contact with
the skin.) This forms the Cu(OH)2 precipitate. After the first 10 drops have been
added, add 10 more drops of 6M NaOH. Centrifuge the solution for 30 seconds
(ask your instructor to operate the centrifuge for you).

2. A Complete Precipitation. Test for a complete precipitation of Cu(OHh by

adding 2-3 more drops of 6M NaOH to the supernatant. (Supernatant: the clear
solution in the test tube). If additional precipitate forms add 4-5 more drops and
again centrifuge. Repeat the test until no further formation of the Cu(OH)2
occurs. The supernatant should appear colorless and the precipitate should be
light blue. Obtain your laboratory instructor's approval and save for Part C.

12
C. Copper(II) Hydroxide to Copper(II) Oxide.

1. Heating to Dryness. Decant (pour off) and discard the supernatant. Carefully
(very carefully!} and slowly heat the test tube with a cool flame until the
Cu(OHh precipitate changes colour. Do not hold the test tube over the direct
flame for a prolonged period. Obtain your instructor's approval and save
for Part D.

D. Copper(II) Oxide to Copper(ll)Sulphate.

1. Dissolution of Copper(II} Oxide. To the solid CuO in the test tube from Part C,
add 20 drops, (1 ml) of 6M H2SO4until the CuO dissolves. (Caution: do not
let sulphuric acid touch the skin!) Slight heating may be necessary, but do it
under supervision! The solution's sky blue appearance is evidence of the
presence of soluble CuSO4. Obtain your instructor's approval and save for Part
E.

E. Copper(II) Sulphate to metallic Copper

1. Formation of Copper Metal. Using fine steel wool, polish about 5-7 cm of Mg
ribbon. Cut or tear the ribbon into 1-cm lengths. Dilute the solution from Part D
with distilled water until the test tube is half full. Add the Mg strips, one at a
time to observe the chemical change, to the solution until the solution is
colorless. Describe exactly what you observe. If a white, milky precipitate forms
(the formation of magnesium hydroxide, Mg(OHh), add several drops of
6M H2S04. (Caution: avoid skin contact!) Break up the red-brown Cu coating
on the Mg ribbon with a stirring rod. Centrifuge the mixture.

2. Washing. Add drops of 6M H2$04 to dissolve any excess Mg ribbon. (Caution:

avoid skin contact!) Do this by breaking up the Cu metal with a stirring rod to
expose the Mg ribbon, coated with Cu metal, to the H2S04 solution. Centrifuge
for 30 seconds decant, and discard the supernatant. Wash the red-brown Cu
metal with three 1-ml portions of distilled water. Centrifuge, decant, and
discard each washing.

3. Determination of the Mass of Recovered Copper Gently dry the Cu in the test
tube over a cool flame. Allow the tube and contents to cool and determine the
mass (±0.001 g). Repeat the heating procedure until a reproducibility in mass
of ± 1% is obtained. Record the mass of Cu recovered in the experiment.
Disposal: All solutions used in the procedure can be disposed of in the sink,
followed by a flush with tap water. Dispose of the copper metal in the "Waste
Solids" container. Check with your instructor. CLEANUP: Rinse all glassware
twice with tap water and once with deionized water. Discard alt rinses in the
sink.

PRE-LABORATORY ASSIGNMENT

I. Define each of the following terms/phrases.

a. decant
b. supernatant
c. "balancing the centrifuge"
d. "cool" flame

13
2. a. At what angle should a test tube be held relative to a Bunsen flame while
heating its contents?

b. What is the typical time interval for centrifuging a sample?

c. What is the minimum number of test tubes needed to operate a centrifuge

properly?

3. Write the correct names and colors of the following chemicals.

FORMULA NAME COLOUR/COLOURLESS

HNO3
H2S04:.
CUD
CU(OH)2:.
CUSO4
CU(N03)2
NAOH
NANO3
NO2
MGSO4

*4. What volume, in drops, of 16 M HNO3 is required to react with 0.020 g of Cu metal?
See first reaction Equation. Assume 20 drops per milliliter. The expression
"16M HNO3" indicates that 16mol HNO3is present in each liter of the HNO3 solution.

REPORT SHEET

Name Data for Copper Sample:

1. Mass of 75-mm test tube (g).

2. Mass of 75-mm test tube+ Cu wool (g).

3. Mass of Cu sample (g).

INSTRUCTOR BALANCED
SYNTHESIS OF OBSERVATION
APPROVAL EQUATION

A. Cu(N03)2
B. Cu(OHh

C. CuO

D. CuS04
E. COPPER(ll)SULPHATE TO COPPER METAL. WRITE A FULL DESCRIPTION OF THE
REACTION THAT OCCURRED. INCLUDE A BALANCED EQUATION IN YOUR
DISCUSSION.

14
4. Mass of test tube + Cu recovered: 1st mass _(g)

2nd mass _(g)

3rd mass _(g).

5. Mass of Cu recovered _(g).

6. Percent recovery: [mass Cu (recovered)/ mass Cu (original)] X 100.

7. Discuss the variance of your percent recovery from the theoretical recovery.

LABORATORY QUESTIONS

1. If the solution remains blue after Part B, but the procedure is continued, how w[[I this
error in the procedure affect the reported percent recovery of copper?

2. If sulphuric acid is not added to dissolve the unreacted Mg metal in Part E.2, will the
reported percent recovery of copper be high or low? Explain.

3. a. Explain what factors may contribute to a greater than 100% recovery of copper
in Part E.3.

b. If the percent recovery of copper in Part E.3 is less than 100%, discuss what
factors may contribute to this error.

15
 EXPERIMENT 4: FORMULA OF A HYDRATE

OBJECTIVES

To determine the percent by mass of water in a hydrated salt. To establish the formula of
a hydrated salt

_.,.._ "'".,.i't iMan sa s occurring in nature or purchased from the grocery shelf or from chemical
hydrated; that is, a number of water molecules are chemically bound to the
-- ons of the salt in its crystalline structure. These water molecules are often referred to as
waters of crystallisation. The number of molecules of water per molecular formula of a salt
is usually a constant. For example, iron(III) chloride is purchased as FeCl3• 6H20,
not as FeCl3, and copper(II) sulphate as CuSO4·5H20, not as CuSO4. For some
salts, the water molecules are so loosely bound to the ions that heat removes them to form
the anhydrous salt. (Anhydrous: without water, esp. water of crystallisation) For Epsom salt
(magnesium sulphate heptahydrate), the anhydrous salt, MgSO4, forms with gentle
heating.

In other salts such as FeCl3·6H20, the water molecules are so strongly bound to the salt
that anhydrous FeCl3 cannot form regardless of the intensity of the heat. In Epsom salt 7
mol of water, or 126.1 g of H20, is bound to each mole of magnesium sulphate, or 120.4 g
of MgSO4. The percent by mass of water in the salt is:

126.lg H O 2 xl00
(126.1g +120.4 g)salt
A gravimetric analysis is an analytical method by which an amount of substance present in
a sample is determined from mass measurements. Generally, the substance being
analyzed must have a mass large enough to be measured easily with the balances that
are available in the laboratory. This experiment uses gravimetric analysis to determine the
percent by mass of water in a hydrated salt and to determine the formula of the hydrated
salt. The sample of a hydrated salt is weighed, and is then heated to drive off the hydrated
water molecules (the waters of crystallization). The mass of remaining sample is measured
again. Cycles of heating and measuring of the sample's mass are continued until mass
reproducibility is attained.

EXPERIMENTAL PROCEDURE

Procedure Overview: The mass of a hydrated salt is measured before and after it is heated
to a high temperature. This mass difference and the mass of the anhydrous salt are the
data needed to calculate the formula of the original hydrated salt. You are to complete
three trials in this experiment. Obtain a hydrated salt from your instructor. Record the
name of the hydrated salt on the Report Sheet.

16
A. Setup for the Gravimetric Analysis

1. Prepare a Clean Crucible.

a. Obtain a clean crucible and lid, support them on a clay triangle, and heat
with an intense flame for 5 minutes. Allow them to cool slowly. (Caution:
do not set them on the lab bench for fear of contamination.) If the
crucible remains dirty after heating, add a few milliliters of 6M HNO3 and
evaporate to dryness. (Caution: avoid skin contact, otherwise wash
immediately under running water)

b. Determine the mass (±0.001 g) of the heated, cold crucible and lid.
Handle the crucible and lid with the crucible tongs for the remainder of
the experiment; do not use your fingers lest oil from the fingers should
contaminate the surface of the crucible and lid. (Handle the crucible with
tongs after heating!)

2. Determine the Mass of Sample. Add no more than 3 g of your hydrated salt to
the crucible and measure the combined mass (±0.001 g) of the crucible, lid,
and sample. Record your data.

3. Adjust the Crucible Lid. Return the crucible (use crucible tongs only!) with the
sample to the clay triangle; set the lid just off the lip of the crucible to allow the
evolved water molecules to escape on heating.

B. Thermal Decomposition of the Sample

I. Heat the Sample. Initially heat the sample slowly and then gradually intensify
the heat. Do not allow the crucible to become red hot. This may cause the
anhydrous salt to decompose as well. Maintain the high temperature on the
sample for 10 minutes. Cover the crucible with the lid; allow them to cool in a
desiccator to room temperature. Determine the combined mass of the crucible,
lid, and sample on the same balance used for earlier measurements.

2. Have you removed all of the water? Reheat the sample for 2 minutes, but do
not intensify the flame-avoid the decomposition of the salt. Again measure the
combined mass. If this second mass measurement of the anhydrous salt
disagrees by greater than ±0.010 g from that in Part B.I, repeat Part B.2.

3. Repeat. Repeat the experiment two more times with an original hydrated salt
sample. Disposal: Dispose of all waste anhydrous salt in the 'Waste Solids"
container. CLEANUP: Rinse the crucible with several milliliters of 1M HCI,
and then rinse several times with tap water and finally deionized water. Each
rinse can be discarded in the sink.

PRE-LABORATORY ASSIGNMENT

1. A 3.211-g sample of gypsum, a hydrated salt of calcium sulfate, CaSO4, is

heated in a crucible until a constant mass is reached. The mass of the
anhydrous CaSO4 salt is 2.539 g.

a. Calculate the percent by mass of water in the hydrated calcium sulfate

salt.

17
 b. Calculate in moles the amount of water removed and in moles the
amount of anhydrous CaSO4 remaining in the crucible.

c. What is the formula of the hydrated calcium sulfate; that is, what is the
whole number mole ratio of calcium sulfate to water?

2. What error in the data is likely to occur if the hydrated salt is heated too
strongly?

3. How long should the hydrated salt initially be heated in removing the hydrated
water molecules? {Read the procedure.)

4. Crucibles and lids are generally handled with crucible tongs in the laboratory.
Why might this be a good technique to acquire?

5. a. What does "firing a crucible" mean?

b. What is the position of the crucible lid when the gaseous products are
allowed to escape from a heated crucible?

REPORT SHEET

NAME OF SALT: TRIAL 1 TRIAL2 TRIAL 3

1. Mass of crucible and lid (g)
2. Mass of crucible, lid and hydrated salt (g)
3. Mass of crucible, lid and anhydrous salt (g)
1st mass (g)
2nd mass (g)
3rd mass (g)
CALCULATIONS
1. Mass of hydrated salt (g)
2. Mass of anhydrous salt (g)
3. Amount of anhydrous salt (mol)
4. Mass of water lost (g)
5. Amount of water lost (mol)
6. Percent by mass of volatile water in hydrated salt
7. Average percent H2O in hydrated salt
, 8. Mole ratio of anhydrous salt to water
9. Formula of the hydrated salt

*Calculations for Trial 1. Show your work.

18
LABORATORY QUESTIONS

1. If some volatile impurities in the crucible are not burned off in Part A.1 but are
removed in Part B.I, is the reported percent mass of water in the hydrated salt too
high or too low? Explain.

2. What happens to the reported percent water if the salt thermally decomposes
yielding a volatile product?

3. If the hydrated water molecules are not completely removed from the salt during the
heating process, will the reported salt-to-water mole ratio be high or low? Explain.

4. Anhydrous calcium chloride, CaCl2, removes water vapor from the air inside a
container having an airtight seal; this laboratory apparatus is called a desiccator.
Discuss how the calcium chloride removes the water vapor.

*5. After heating the crucible in Part A.I, the crucible is set on the lab bench where it is
contaminated with the cleaning oil used to clean the lab bench before its mass is
measured. The analysis continues through Part B.I where the mass of the anhydrous
salt is determined. In the heating the cleaning oil is burned off the bottom of the
crucible. Describe the error that has occurred; that is, is the mass of the anhydrous
salt remaining in the crucible reported as being too high or too low? Explain.

19
EXPERIMENT 5: LIMITING REAGENT

OBJECTIVES

To determine the limiting reactant in a salt mixture.

To determine the percent composition of each substance in a salt mixture.

INTRODUCTION

Two factors affect the yield of products in a chemical reaction: (1) the amounts of starting
materials (reactants) and (2) the percent yield of the reaction. Many experimental
conditions, for example, temperature and pr, ssure, can be adjusted to increase the yield
of a desired product in a chemical reaction, but because chemicals react according to fixed
mole ratios (stoichiometrica/ly), only a limited amount of product can form from given
amounts of starting materials. The reactant determining the amount of product generated
in a chemical reaction is called the limiting reactant in the chemical system. (Percent
composition: the mass ratio of the components of a mixture or compound to the total mass
of the sample.

Percent yield: [actual yield/theoretical yield] x100

Stoichiometrically: by a study of a chemical reaction using a balanced equation). To better

understand the concept of the limiting reactant, let us look at the reaction under
investigation in this experiment, the reaction of sodium phosphate dodecahydrate,
Na3P04·12H20, and barium chloride dihydrate, BaCl2·2H20, in an aqueous system. The
molecular form of the equation for the reaction is

As the two reactant salts and sodium chloride are soluble in water but barium phosphate is
insoluble, the ionic equation for the reaction is:

6Na+(aq) + 2POi-(aq) + 3Ba2+(aq) + 6Cr(aq) + 30H2O(I)

Ba3(PO4h(s) + 6 Na+(aq) + 6 Cl"(aq) + 30 H2O(I)

Presenting only the ions that react (and removing the spectator ions), we have the net
ionic equation.

The balanced net ionic equation dictates that, 2mol of the phosphate ion react with 3mol of
barium ion. The equation also predicts the formation of

1 mol of Ba3(PO4)2.(1 mol of Na3PO4·12H20, mass= 380.2g, therefore 2 mol corresponds

to 760.4g); (1 mol of BaCl2·2H2O, mass= 244.2g, therefore 3 mol corresponds to 732.6g);
(1 mol of Ba3(PO,1}2, mass = 601.96g). ( Note: Gravity filtration is used to filter finely
divided precipitates.).

20
In this experiment, the salts Na3PO4·12H2O and BaCl2·2H2O form a heterogeneous
mixture of unknown composition. The masses of the constituent salts of the initial salt
mixture are measured. The mixture is added to water and the insoluble Ba3(PO4)2 forms.
The mass of the Ba3(PO4h precipitate is measured. The percent composition of the salt
mixture is determined by first testing for the limiting reactant. The limiting reactant, in the
formation of the barium phosphate, is determined from two precipitation tests of the
solution: the solution is tested for an excess of barium ion with a phosphate reagent;
observed formation of a precipitate indicates the presence of an excess of barium ion (and
a limited amount of phosphate ion) in the salt mixture; the solution is also tested for an
excess of phosphate ion with a barium reagent; observed formation of a precipitate
indicates the presence of an excess of phosphate ion (and a limited amount of barium ion)
in the salt mixture.

CALCULATIONS

The calculations required for the analysis of the data in this experiment are involved. The
question, after collection of all of the data becomes, "How do I proceed to determine the
percent composition of a salt mixture containing the salts Na3PO4·12H2O and BaC'2·2H2O
from the data of a precipitation reaction?"

Consider the following example:

A 0.942-g sample of the salt mixture is added to water and 0.188 g of Ba3(PO4)zprecipitate
forms. Tests reveal that BaCl2·2H2O is the limiting reactant. What is the percent
composition of the salt mixture? The amount of BaCl2•2H2O determines the amount of the
product generated because BaCl2• 2H2O is the limiting reactant. Further, the stoichiometry
of the net ionic equation indicates that to form 1 mol Ba3(PO4)2 precipitate 3 mol Ba2+ is
required (and therefore 3 mol BaCl2·2H2O). Therefore, the amount of Ba3(PO4)2 is given by
the mass divided by the molar mass. (0.188 g Ba3(PO4)z}/601.96gmor1 = 3.12 x 10-4mol
The amount of Ba2+ required is three times as much, which is 9.37 x 10-4 mol. In turn, the
mass of BaCl2·2H2O is given by the amount times the molar mass.

(9.37 x 10-4 mol BaCl2·2H2O x 244.2g/mol) = 0.229g

The total mass of the initial salt mixture is 0.942g, which means the mass of
Na3PO4·12H2O is 0.713g. The percent BaC'2-2H2O in the salt mixture
is:(0.229 g / 0.942 g) x 100 = 24.3%. The percent Na3PO4· 12H2O in the salt mixture is:
(0.713 Q / 0.942 g) X 100 = 75.7%.

EXPERIMENTAL PROCEDURE

Procedure Overview: A measured mass of a salt mixture of unknown composition is added

to water. The precipitate that forms is digested, filtered, and dried, and its mass measured.
Observations from tests on the supernatant solution determine which salt in the mixture is
the limiting reactant. An analysis of the data provides the determination of the percent
composition of the salt mixture. Three trials will be done for this experiment. To hasten the
analyses, measure the masses of samples of unknown salt mixtures and simultaneously
follow the procedure for each. Label the beakers accordingly to avoid the intermixing of
samples and solutions. Obtain an unknown Na3PO4·12H2O/ BaCl2·2H2O salt mixture from
your instructor.

21
A. Precipitation of Ba3(PO4)2 from the salt

1. Prepare the Salt Mixture.

a. Measure (±0.001 g) on weighing paper about 1 g of the salt mixture.

Record this mass for Trial 1 on the Report Sheet. Repeat for Trial 2 and
3.

b. Transfer the salt mixture to a labelled 400-mL beaker and add 200 ml
(±0.2 ml) of deionised water. Stir the mixture with a stirring rod for about
1 minute and then allow the precipitate to settle. Leave the stirring rod in
the beaker.

2. Digest the Precipitate.

Cover the beaker with a watchglass and maintain the solution hot (80-90°C) on
a steam bath or with a low, cool flame for 30 minutes. (This is called digesting
the precipitate. This heating procedure causes the formation of larger
Ba3(PO4)2 particles.) While the precipitate is being kept warm, proceed to Part
A.3. Periodically check on the progress of the heating. After 30 minutes,
remove the heat, and allow the precipitate to settle; the solution does not need
to cool to room temperature. While the precipitate is settling, heat in a 150-ml
beaker, about 30 ml of deionised water for use as wash water in Part A.5.

3. Set Up a Gravity Filtering Apparatus. Place your initials (in pencil) on a piece of
Whatman No. 42 or Fisherbrand Q2 filter paper and detennine its mass
(±0.001 g). Fold it properly and seal it into the filter funnel with a small amount
of deionized water. Discard the water in the receiving flask. Have your
instructor inspect your apparatus before continuing. Return to Part A.2b.

4. Decant the Supernatant. Once the supernatant has cleared in Part A.2b, use a
50-ml graduated cylinder to decant two 50-ml (±0.2 ml) volumes into
separate 100-ml beakers, labelled Beaker I and Beaker II. Save for Part B.
(Note: Whatman No. 42 and Fisherbrand Q2 filter papers are both fine-porosity
filter papers; a fine-porosity filter paper is required to filter the finely divided
8a3(PO4)2 precipitate.)

5. Filter the Ba3(PO4)2 Precipitate. While the solution from Part A.4 is still warm,
quantitatively transfer the precipitate to the filter. Remove any precipitate on
the wall of the beaker with a rubber policeman; wash any remaining precipitate
onto the filter with several 5-ml volumes of warm (80-90°C) water (from Part
A.2b). Wash the Ba3(PO4)z precipitate on the filter paper with two additional 5-
ml portions of warm water.

6. Dry and Measure the Amount of 8a3(PO4)2Precipitate. Remove the filter paper
and precipitate from the filter funnel. Air-dry the precipitate on the filter paper
until the next laboratory period or dry in a 110°C constant temperature drying
oven overnight. Determine the combined mass (±0.001 g) of the precipitate
and filter paper. Record.

B. Determination of the Limiting Reactant

From the following two tests you can determine the limiting reactant in the original
salt mixture. Some cloudiness may appear in both tests, but one will show a definite
fonnation of precipitate.
22
 1. Test for Excess Poi-. Add 2 drops of 0.5 M Ba2+ (from 0.5 M BaCl2) to the 50
ml.'.::of ·supernatant liquid in Beaker I. If a precipitate forms, the P043- is in
excess and Ba2+ is the limiting reactant in the original salt mixture.

2. Test for Excess Ba2+_ Add 2 drops of 0.5 M Poi- (from 0.5 M Na3P04) to the
50 ml of supernatant liquid in Beaker II. If a precipitate forms, the Ba2+ is in
excess and P043- is the limiting reactant in the original salt mixture.

Disposal: Dispose of the barium phosphate, including the filter paper, in the
'Waste Solids" container. Dispose of the waste solutions in the "Waste Liquids"
container. CLEANUP: Rinse each beaker with small portions of warm water
and discard in the "Waste Liquids" container. Rinse twice with tap water and
once with deionised water and discard in the sink.

PRE-LABORATORY ASSIGNMENT

1. a. What does the expression, "digesting a precipitate" mean?

b. Describe the procedure for digesting a precipitate.

2. a. Describe in your own words how the mass of Ba3(P04)2precipitate is determined

in Part A.

b. Describe how to test your unknown salt mixture for the presence of excess
Na3P04·12H20.

3. The Ba3(P04)2(molar mass = 601.96 g/mol) precipitate that forms from a salt mixture
has a mass of 0.194 g. Experimental tests revealed that Na3P04•12H20
(molar mass= 380.2 g/mol) was the limiting reactant in the fonnation of the
precipitate and that BaC'2· 2H20 was the excess reactant in the salt mixture.
Determine the mass of Na3P04·12H20 (molar mass = 380.2 g/mol) in the salt
mixture.

4. When 0.629 g of Na3P04· 12H20 (molar mass = 380.2 g/mol) and 0.527 g of
BaCl2• 2H20 (molar mass = 244.2 g/mol} are mixed with water forming 500 ml of
solution, how many grams of Ba3(P04)2 (molar mass= 601.96 g/mol) precipitates?

5. Why is fine-porosity filter paper required for use in the filtering of the Ba3(P04h
precipitate?

23
REPORT SHEET

A. Precipitation of Ba3(P04h from the Salt Mixture

Sample no.: Trial 1 Trial2 Trial 3

1. Mass of salt mixture (g)

2. Mass of filter paper (g)

3. Mass of filter paper and Ba3(P04)2(g)

4. Mass of Ba3(P04)2 (g)

8. Determination of Limiting Reactant

1. Limiting reactant in salt mixture (write complete formula)

2. Excess reactant in salt mixture (write complete formula)

Calculations

I. Amount in moles of Ba3(P04)2precipitated (mol)

2. Amount in moles of limiting reactant in salt mixture (mol)

Formula of limiting hydrate

3. Mass of limiting reactant in salt mixture (g)

Formula of limiting hydrate

4. Mass of excess reactant in salt mixture (g) ,

Formula of excess hydrate

5. Percent limiting reactant in salt mixture(%)

Formula of limiting hydrate

6. Percent excess reactant in salt mixture (%)

.

Formula of excess hydrate

Show Calculations for Trial 1.

24
LABORATORY QUESTIONS

1. Because Ba3(PO4)2 is a very finely divided precipitate, some is lost in :the filrerin·g
process. As a result is the reported "percent limiting reactant" high or low? Explain.

2. Because of the slight solubility, 0.519 mg/L, of Ba3(PO4)2, all of the Ba2 .. and Po/·
ions do not precipitate from solution.

a. What mass in milligrams and amount in moles of Baa(PO4)2 dissolve in 200 ml

of solution?

b. How does this loss affect the reported "percent excess reactant" in the original
salt mixture? Explain.

3. According to your data, how many grams of the excess reactant participated in the
reaction and how many grams did not?

* 4. If Na2SO4 is an unknown contaminant of Na3PO4·12H2O, how does its presence

affect the yield of Ba3(PO4)2in the experiment? BaSO4 is also insoluble.

25
EXPERIMENT 6 : PERIODIC TABLE AND PERIODIC LAW

OBJECTIVES

1. To become more familiar with the periodic table.

2. To predict trends in various atomic properties within groups and periods of elements.
3. To observe from experiment the trends in the chemical properties within groups and
periods of elements.

INTRODUCTION

Similarities between the chemical and physical properties of the elements were known
early in the nineteenth century. It remained until 1869, for two scientists, Dmitri Mendeleev
from Russia and Lothar Meyer from Germany, to independently establish a periodic table
similar to our present-day arrangement of the elements. Mendeleev showed that with the
elements arranged in order of increasing atomic mass, their chemical properties recur
periodically. When Meyer arranged the elements in order of increasing atomic mass, he
found that their physical properties recur periodically. The two tables, however, were
virtually identical. Because he drafted his table earlier in 1869 and because his table
included "blanks" for yet-to-be-discovered elements to fit, Mendeleev is considered the
"father of the modern periodic table." In 1913, H.G.J. Moseley's study of the X-ray spectra
of the elements refined the periodic table to its current status: when the elements are
arranged in order of increasing atomic number, certain chemical and physical properties
repeat periodically. In the periodic table, each horizontal row of elements is called a period
and each column is a group. All elements within a group have similar chemical and
physical properties. Common terms associated with various sections of the periodic table
are:

• Representative elements: Group "A" elements.

• Transition elements: Groups 3-11.
• Inner transition elements: the lanthanide and actinide series.
• Metallic elements: elements to the left of the "stairstep line" that runs diagonally from B
to At.
• Nonmetallic elements: elements to the right of the "stairstep line".
• Metalloids: elements that lie adjacent to the "stairstep line," excluding Al.
• Alkali metals: Group IA elements
• Alkaline earth metals: Group IIA elements
• Chalcogens: Group VIA elements
• Halogens: Group VIIA elements • Noble gases
• Rare earth metals: the lanthanum series of elements
• Coinage metals: Cu, Ag, Au
• Noble metals: Ag, Au, Pt, Pd, Hg, Rh, Ir, Ru, Os

The periodicity of a physical property for a series of elements can be shown by plotting the
experimental value of the property against increasing atomic number. Physical properties
studied in this experiment are:

• Electronegativity: the degree to which an atom in a molecule attracts electrons in a

chemical bond.
• Atomic radius: the radius of an atom of the element.

26
• Electron affinity: the energy released when a neutral gaseous atom accepts an
electron.
• Ionization energy: the energy required to remove an electron from a gaseous atom.
• Melting point: the temperature at which the solid and liquid phases of a substance
coexist.
• Boiling point: the temperature at which the vapor pressure of the liquid equals one
atmosphere.
• Molar volume: the volume of a unit cell times Avogadro's number divided by the
number of atoms in the unit cell

Trends in the chemical properties of the following elements are also studied in this
experiment.

Na Mg Ca Al S Cl Br I

In this experiment, the relative acidic and/or basic strength of hydroxides or oxides in the
third period of the periodic table, the relative chemical reactivity of chlorine through iodine,
and the relative solubility of the hydroxides of magnesium and calcium are observed
through a series of qualitative tests. Observe closely the results of each test before
generalizing your information.

EXPERIMENTAL PROCEDURE

Procedure Overview: General trends in the physical properties of elements listed in the
Table provided are observed from three kinds of data plots. Experimental observations of
the physical and chemical properties of a number of representative elements are made.
Special attention is paid to the chemical properties of the halogens.

A. The Appearance of Some Representative Elements

1. Samples of Metallic Elements. Samples of sodium, magnesium, aluminum.

silicon, and sulfur are on the reagent table. Note the Na metal is stored under a
nonaqueous liquid to prevent any rapid air oxidation. Polish the Mg and Al
metal strips with steel wool for better viewing. Record your observations on the
Report Sheet.

2. Chlorine. In test tube A1 of a set of test tubes, place 10 drops of a 5 % sodium

hypochlorite, NaCIO, solution (commercial laundry bleach) and 2 drops of
mineral oil. Which layer is the mineral oil layer? Add 10 drops of 6M HCI
(Caution: 6M HCI is very corrosive. Avoid contact with skin or else wash
affected area immediately under running water). Swirl/agitate (with a stirring
rod) the mixture so that the HCI mixes with the NaCIO solution. Note the colour
of the chlorine in the mineral oil layer.

3. Bromine. In test tube A2, place 10 drops of a 6M KBr solution and 2 drops of
mineral oil. Add 5 drops of concentrated sulfuric acid (Caution: concentrated
H 04 attacks skin tissue; flush the affected area immediately with water.)
Agitate/swirl the mixture so that the concentrated H2S04 mixes with the KBr
solution. Note the colour of the mineral oil layer.

4. Iodine. Repeat Part C.3 in well A3, substituting 6M Kl for 6 M KBr.

27
B. The Chemical Properties

1. Chlorine and its Reactions with the Bromide and Iodide Ions. To well 81 add a
few crystals (use tip of a spatula) of solid KBr and to well B2, a a few crystals
of solid Kl. Add 10 drops of a 5 % sodium hypochlorite, NaCIO, solution, 5
drops of 6M HCI, and 2 drops of mineral oil to each well. Swirl/agitate with a
stirring rod and observe.

2. Bromine and its Reactions with the Chloride and Iodide Ions. To well B3 add a
few crystals of solid NaCl and to well B4, a few of solid Kl. Add 10 drops of 6M
KBr, 5 drops of concentrated H2S04 (Caution!), and 2 drops of mineral oil to
test tubes B3 and B4. Swirl/agitate with a stirring rod and observe.

3. Iodine and its Reactions with the Chloride and Bromide Ions. To a few crystals
of solid NaCl and to well B6, a few crystals of solid KBr. Add 10 drops of 6M Kl,
5 drops of concentrated H2SO4 (Caution!), and 2 drops of mineral oil to test
tubes B5 and B6. Swirl/agitate with a stitring rod and observe.

4. The Reactions of the Halides with Various Metal Ions. Prepare a set of test
tubes as follows:

Test tubes C1-C3, a pinch of NaF and 10 drops of water.

Test tubes C4-C6, a pinch of NaCl and 10 drops of water.
Test tubes D1-D3, a pinch of KBr and 10 drops of water.
Test tubes D4-D6, a pinch of Kl and 10 drops of water.

Slowly add 10 drops of 2M Ca(NO3)2 to test tubes C1, C4, D1, and D4.
Observe closely and over a period of time. Slowly add 10 drops of 0.1 M
AgNO3 to test tubes C2, CS, D2, and D5. After about 1 minute, add 10 drops of
3 M NH3 to test tubes C2, C5, D2, and 05. Add 1 drop of 6 M HNO3 and
slowly add 10 drops of 0.1 M Fe(NO3)3 to test tubes C3, C6, D3, and D6.
Observe closely and over a period of time. Disposal: Dispose of the waste
water/halogen mixtures in the "Waste Halogens" container. CLEANUP: Rinse
the test tubes with copius amounts of tap water and twice with deionized water.
Discard the rinses in the sink.

C. Chemical Reactivity of Some Representative Elements

1. Sodium. Instructor Demonstration Only. Wrap a pea-size piece of sodium

metal in aluminum foil. Fill a 200-mm Pyrex test tube with water, add 2 drops of
phenolphthalein, (an acid-base indicator, colorless in an acidic solution but pink
in a basic solution) and invert it in a beaker of water. Set the beaker and test
tube behind a safety shield. Punch 5-10 holes with a pin in the aluminum foil.
With a pair of tongs or tweezers, place the wrapped sodium metal in the mouth
of the test tube, keeping it under water. What is the evolved gas? Test the gas
by holding the mouth of the inverted test tube over a Bunsen flame. A loud
"pop" indicates the presence of hydrogen gas. Account for the appearance of
the color due to phenolphthalein.

2. Magnesium and Aluminium. Add 10 drops of 3M HCI (Caution: Do not allow

it to touch the skin; wash the affected area immediately.) to test tubes A1-A2 of
a set of test tubes. Polish strips of Mg and Al metal; cut 5 mm pieces and place
them into separate test tubes. Which metal reacts more rapidly? What is the
28
 gas that is evolved? Add (and count!) drops of 6 M NaOH to each well until a
precipitate appears. Continue to add NaOH to test tube A2 (containing the
aluminum ion) until the precipitate dissolves. (Magnesium ion precipitates as
magnesium hydroxide, Mg(OH)2; aluminium ion also precipitates as the
hydroxide, Al(OH)J, but redissolves in an excess of OH to produce Al(OH)/,
the aluminate ion.) Add the same number of drops to test tube A1. Record your
observations.

3. Hydroxides of Magnesium and Calcium. Place 10 drops of 0.10 M MgCl2 in test

tube 81 and 10 drops of 0.10 M CaCl2 in test tube B2. Count and add drops of
0.010 M NaOH until a cloudiness appears in each. Predict the trend in
solubility of the hydroxides of the Group IIA cations.

4. Sulfur Dioxide and Sulfuric Acid. Place a few crystals of solid sodium sulfite,
Na2SO3, in test tube C1. Add 5 drops of 6 M HCI. Test the evolved gas with
wet, blue litmus paper. Write a balanced equation for the reaction. Test 5
drops of 0.1 M H2SO4 in test tube C2 with litmus paper, both by holding
moistened, blue litmus paper over the well and by a direct test of the solution.
Disposal: Discard the solutions from the well plate in the sink, followed by a
flush with tap water. CLEANUP: Rinse the well plate with tap water twice and
with deionized water once. Discard the rinses in the sink.

PRE-LABORATORY ASSIGNMENT

On the blank periodic table, clearly locate the following, using your own color code.

a. Representative elements.

Transition elements
Chalcogens
Alkali metals
Alkaline earth metals
Halogens
Noble gases

2. On the same periodic table, locate these elements and write in their correct atomic
symbols.

a. sodium k. aluminum
b. bromine I. argon
c. calcium m. nickel
d. potassium n. magnesium
e. chlorine 0. silicon
f. fluorine p. iodine
g. phosphorus q. uranium
h. barium r. sulfur
i. lead s. zinc
j. carbon t. gold

29
3. The chemical reactivity of three halogens are studied in this experiment. Name them
and write formulas for their naturally occurring molecules.

a.
b.
C.

4. a. When proceeding from left to right across a period in the periodic table, the
elements become (more/ less) metallic.
b. When proceeding from top to bottom in a group, the elements become (more/
less) metallic.

REPORT SHEET

A. The Appearance of Some Representative Elements

PHYSICAL PHYSICAL
ELEMENT COLOUR
STATE APPEARANCE
Na
Mg
Al
Si
Ss
Cl2
b

B. The Chemical Properties of the Halogens

REACTION OBSERVATION EQUATION

Cl2 + Br"
Cl2 + r
Br2 + Cr
Br2 + r
12 + er
12 + Br"

What can you conclude about the reactivity of Cl2, Br2, and 12

30
C. The Reactions of the Halides with Various Metal Ions

Ca(NO3)2(aq) AgNOa(aq) Fe(NO3h(aq)

NaF(aq)
NaCl(aq)
NaBr(aq)
Nal(aq)

Describe the appearance of each mixture

D. Chemical Reactivity of Some Representative Elements

1. Sodium.

a. Gas evolved in the reaction of Na with water.

b. What product is produced from the reaction of Na with water as indicated

by the action of phenolphthalein?

c. Chemical equation for the reaction of Na with water.

2. Magnesium and Aluminum

a. Which metal reacts more rapidly with HCI?

b. What is the gas that is evolved when Mg and A1 react with HCI?
c. Reaction of metal ion with limited amount of NaOH:

Mg observation (Drops to precipitate)

Al observation (Drops to precipitate)

Reaction of metal hydroxide with an excess of NaOH:

Mg observation
Al observation

c. Explain the differences in chemical behavior of the magnesium and aluminum

hydroxides. Use chemical equations in your discussion.

Hydroxides of Magnesium and Calcium

Mg observation (Drops to precipitate)

Ca observation (Drops to precipitate)
Which OH- salt is most soluble? Least soluble?

What can you conclude about the trend in solubilities of the Group IIA metal
hydroxides?

31
4. Sulfur Dioxide and Sulfuric Acid.

Equation for the generation of S02(g).

What does the litmus test indicate about the chemical nature of S02(g)?

What is the color of the litmus paper in a H2S04 solution?

What differentiates sulfurous acid from sulfuric acid?

LABORATORY QUESTIONS

Review your data and the relationships that were established in this experiment to answer
the following questions.

1. Complete the following statements with the correct word(s).

a. Paralleling an increase in atomic number within a period of elements there is a

general in ionization energy.

b. An increase in the atomic number within a period of elements is accompanied by

a general in the atomic radii.

c. The ionization energy within a group of representative elements

with increasing atomic radii.

d. The group of representative elements that has the highest melting points is
Group

e. The group of representative elements that has the lowest boiling points is Group

f. The element that has the highest electronegativity is

g. The electronegativity of elements within a period with

increasing ionization energy.

h. The atomic radii of elements within a period with increasing

electronegativity.

i. An increase in the atomic number within a group of representative elements is

accompanied by a general in electronegativity.

2. When the elements are arranged in order of increasing atomic ------

certain chemical and physical properties repeat periodically. Describe the general
trend in physical appearance of the elements in Period 3, in Group VIIA. Which
halogen is most reactive? least reactive? What observations justify your predictions?

3. How does the reactivity of the metals vary across a period (left to right) of elements?
What observations justify your predictions?

32
EXPERIMENT 7: A VOLUMETRIC ANALYSIS

OBJECTIVES

To prepare and standardize a sodium hydroxide solution

To determine the molar concentration of a strong acid

INTRODUCTION

A chemical analysis that is performed primarily with the aid of volumetric glassware (e.g.,
pipettes, burettes, volumetric flasks) is called a volumetric analysis. An aqueous solution
containing an unknown substance can be analyzed by reacting it with a very well known
amount in moles of a second reactant. A procedure in which an accurately measured
volume of a standard solution containing a reactant is carefully added until all of an
unknown substance reacts is known as a titration. (Standard solution: a solution having a
very well known concentration of a substance) The titration procedure requires a buret to
dispense a liquid, called the titrant into a flask containing the analyte. The titrant may be a
solution of amounts known or unknown concentration. The analyte may be a solution with
a volume measured with a pipet or it may be a dissolved solid with a very accurately
measured mass. A reaction is complete when stoichiometric amounts of the reacting
substances are combined. (Stoichiometric amounts: amounts corresponding to the
balanced equation) This is the stoichiometric point in the titration. In this experiment the
stoichiometric point for an acid-base titration is detected using a phenolphthalein indicator.
Phenolphthalein is an acid-base indicator, colorless in an acidic solution but pink in a basic
solution. The point in the titration at which the phenolphthalein changes color is called the
endpoint of the indicator. Indicators are selected so that the stoichiometric point in the
titration coincides (at approximately the same pH) with the endpoint of the indicator.

Part A : Standardization of a sodium hydroxide solution

Solid sodium hydroxide is very hygroscopic(absorbs water vapor readily); and therefore, its
mass cannot be accurately measured. To prepare a NaOH solution with a more exact
molar concentration, it must be standardized with an acid that is a primary standard.
(Primary standard: a substance primary standard because of its high purity and relatively
high molar mass and is non-hygroscopic). Part A of this experiment, dry potassium
hydrogen phthalate, KHC8H4O4, is used as the primary acid standard for determining the
molar concentration of a sodium hydroxide solution. Potassium hydrogen phthalate has the
properties of a primary standard because of its high purity and relatively high molar mass
and because it is not hygroscopic. The amount of KHC8H4O4, n (mol), used for the analysis
is calculated from its measured mass m (g), and molar mass (M "" 204.2 g/mol).

n [mol] = m [g] + M [g/mol] (1)

From the balanced equation for the reaction, one mole of KHC8H4O4 reacts with one mole
of NaOH.

(2)

In the experimental procedure an accurately measured mass of dry potassium hydrogen

phthalate is dissolved in deionized water. A prepared NaOH solution is then dispensed
from a buret into the KHC8H4O4 solution until the stoichiometric point is reached, which is
signaled by the change of the phenolphthalein indicator from colorless to pink. At this point
the dispensed volume of NaOH is noted and recorded(!).
33
The molar concentration (c)of the NaOH solution in (mol/L)is calculated as

c [mol/Ll = n [mol] +Volume of solution (L) (3)

taking reaction equation (1), into consideration.

Part B : Molar Concentration of an Acid Solution

In Part B, an unknown molar concentration of an acid solution is determined. The

standardized NaOH solution, now called a secondary standard, is used to titrate an
accurately measured volume of the acid to the stoichiometric point. By knowing the volume
(V), and molar concentration (c) of the NaOH, the amount (n) of the base used in the
analysis is

V [Ll i2i c [mol/Ll = n [mol]

From the stoichiometry of the reaction the amount of acid neutralized in the reaction can
be calculated. From the measured volume and the amount of the acid that react, the
molar concentration of the acid is calculated.

EXPERIMENTAL PROCEDURE

Procedure Overview: A NaOH solution is prepared with an approximate concentration. A

more accurate molar concentration of the NaOH solution (as the titrant) is determined
using dry potassium hydrogen phthalate as a primary standard (titrand). The NaOH
solution, now a secondary standard solution, is then used to determine the molar
concentration of an acid solution.

A. The Standardization of a Sodium Hydroxide Solution

You are to complete at least three "good" trials (±1% reproducibility) in standardizing
the NaOH solution. Prepare three clean 125-ml or 250-ml Erlenmeyer flasks for the
titration. You will need to use approximately one liter of boiled, deionized water for
this experiment. Start preparing that first.

1. Prepare the Stock NaOH SoluUon. One week before the scheduled laboratory
period, dissolve about 4 g of NaOH (pellets or flakes) in 5 ml of deionized water
in a 150-mm rubber-stoppered test tube. Thoroughly mix and allow the solution
to stand for the precipitation of sodium carbonate, Na2CO3.

2. Dry the Primary Standard Acid. Dry 2-3 g of KHC0H4O4 at 110°C for several
hours in a constant temperature drying oven. Cool the sample in a desiccator.

3. Prepare the Diluted NaOH Solution. Decant about 4 ml of the NaOH solution
prepared in Part A.1 into a 500-ml polyethylene bottle. (Caution: concentrated
NaOH solution causes severe skin removal!) Dilute to 500 ml with previously
boiled,(boiling removes traces of CO2) deionized water. Cap the polyethylene
bottle to prevent the absorption of CO2. Swirl the solution and label the bottle.
Calculate an approximate molar concentration of your diluted NaOH solution.

34
 4. Prepare the Primary Standard Acid. Calculate the mass of KHC8H404 that will
require about 15-20 ml of your diluted NaOH solution to reach the
stoichiometric point. Measure this mass (±0.001 g) of KHC8H404 on weighing
paper and transfer it to the Erlenmeyer flask. Similarly, prepare all three samples
while you are occupying the balance. Add about 50 ml of previeusly boiled,
deionized water and 2 drops of phenolphthalein.

5. Prepare a Clean Surette. Wash a 50-ml burette and a funnel thoroughly with
soap and water using a long burette brush. Flush the burette with tap water and
rinse several times with deionized water. Rinse the burette with three 5ml
portions of the diluted NaOH solution, making certain that the solution wets the
entire inner surface. Drain each rinse through the burette tip. Have the instructor
approve your titration apparatus before continuing.

6. Fill the Surette. Using a clean funnel, fill the burette with the NaOH solution.
After 30 seconds, read the volume (±0.02 ml) by viewing the bottom of the
meniscus with the aid of a black line drawn on a white card. Record this initial
volume. Place white paper beneath the Erlenmeyer flask.

7. Titrate the Primary Standard Acid. Slowly add the NaOH solution from the
burette to the acid, swirling the flask (with the proper hands) after each addition.
Initially, add the NaOH solution in 1 to 2 ml increments. Occasionally rinse the
wall of the flask with (previously boiled, deionized) water from your wash bottle.
As the endpoint nears, the color of the indicator disappears gradually. Continue
addition of the NaOH titrant until the endpoint is reached. The endpoint in the
titration should be within one-half drop of a slight pink color. The color should
persist for 30 seconds. Read and record the final volume of NaOH in the burette.

8. Repeat the Analysis with the Remaining Standard Acid Samples. Refill the
burette and repeat the titration at least three more times with varying, but
accurately known, masses of KHC8H4O4.

9. Do the Calculations. Calculate the molar concentration of the diluted NaOH

solution. The molar concentrations of the NaOH solution from three analyses
should be within ±1%. Place a corresponding label on the 500-ml polyethylene
bottle. Disposal: Dispose of the neutralized solutions in the Erlenmeyer flasks
in the 'Waste Acids" container.

8. Molar Concentration of an Acid Solution

Three samples of the acid having an unknown concentration are to be analyzed. Ask
your instructor for the type of your unknown acid (i.e., HA, H2A, or H:A). Prepare
three clean 125 or 250 ml Erlenmeyer flasks for this determination.

1. Prepare the Unknown Acid Samples. In an Erlenmeyer flask, pipette 25 ml of

the acid solution. Add 2 drops of phenolphthalein.

2. Fill the Surette and Titrate. Refill the burette with the (now) standardized NaOH
solution and after 30 seconds, read and record the initial volume. Refer to Parts
A.6 and A.7. Titrate the acid sample to the phenolphthalein endpoint. After 30
seconds, read and record the final volume of titrant.

3. Repeat. Similarly titrate the other samples of the acid solution.

35
 4. Save. For further use save your standardized NaOH solution in the tightly
capped 500-ml polyethylene bottle. Disposal: Dispose of the neutralized
solutions in the "Waste Acids" container. Consult with your instructor.
CLEANUP: Rinse the burette several times with tap water and discard through
the tip into the sink. Rinse twice with deionized water. Similarly clean the
Erlenmeyer flasks. Check and clean the balance area. All solids should be
discarded in the "Waste Solids" container.

PRELABORATORY ASSIGNMENT

1. Distinguish between a stoichiometric point and an endpoint.

2. a. Name and write the formula of the primary standard that is used for
standardizing the NaOH solution in this experiment.

b. Write a balanced equation, showing its reaction with NaOH.

3. Potassium hydrogen phthalate is not hygroscopic. What does that mean?

4. Describe how one-half drop of titrant can be added from a burette.

5. a. A 0.394-g sample of potassium hydrogen phthalate, KHCaH4O4, is dissolved in

100 ml of water. If 13.93ml NaOH solution is required to reach the
stoichiometric point, what is the molar concentration of the sodium hydroxide
solution? The molar mass of KHC8H4O4is 204.2 g/mol.

b. Oxalic acid, H2C2O4·2H20 (molar mass 126.07 g/mol), can also be used as a
primary standard for the standardization of a NaOH solution. What mass of
oxalic acid would be needed for the reaction of the 13.93 ml of NaOH used in
a? Hint: Oxalic acid is an H2A (diprotic) acid.

6. A 25.00ml volume of a diprotic acid solution of unknown concentration with 2 drops

of phenolphthalein requires 13.40 ml of 0.1320 M NaOH to reach the endpoint.

a. What will be the color change at the endpoint?

b. What is the molar concentration of the acid solution?

Maintain at least three significant figures when recording data and performing
calculations.

REPORT SHEET

A. Standardization of a Sodium Hydroxide Solution

1. Approximate molar concentration of diluted NaOH solution. Show calculations.

2. Approximate mass of KHC8H4O4 for the standardization of the NaOH solution.
Show calculations.

36
 Trial 1 Trlal 2 Trial 3
I. Mass of flask and KHCeH4Q4 (g)
2. Mass of flask (g)
3. Mass of KHCaH4Q4 (g)
4. Molar mass of KHCsH4Q4 204.2 g/mol
5. Amount of KHCsH4O4 (mol)
Titration apparatus approval
6. Burette reading of NaOH, final (ml)
7. Surette reading NaOH, initial (ml)
I
8. Volume of NaOH dispensed (ml)
9. Molar concentration, NaOH (mol/1)
10. Average molar concentration NaOH (mol/I)

B. Molar Concentration of an Acid Solution

Acid type: Unknown Sample Sample Sample

No. 1 2 3
1.Volume of acid solution (ml) 25.0 25.0 25.0
2. Surette reading NaOH, final {ml)
3. Surette reading NaOH, initial (ml)
4. Volume of NaOH dispensed (ml) I

5. Molar concentration of NaOH (mol/L), Part A

6. Moles of NaOH dispensed (mol)
7. Molar concentration of acid solution (mol/L)
8. Average molar concentration of acid solution (mol/L)

* Show calculations for Sample 1!!!!!!l!!

LABORATORY QUESTIONS

1. Explain why it is quantitatively not acceptable to titrate all of the KHC8H4O4 samples
with the NaOH solution to the same dark red endpoint.

2. If the endpoint in the titration of the KHC8H4O4 solutions with the NaOH solution is
mistakenly surpassed (too pink), will the molar concentration of the NaOH solution
be reported too high or too low? Explain.

37
3. If, in Part A, a drop of NaOH solution is dispensed from the buret but adheres to the
side of the Erlenmeyer flask during its standardization, how will this affect:

a. The reported molar concentration of the NaOH solution?

b. The reported molar concentration of the unknown acid solution in Part B?

4. In Part A, if an air bubble is originally trapped in the buret tip but disappears during
the titration, will the reported molar concentration of the NaOH solution be too high or
too low? Explain.

*5. "If 2 drops are good, 20 drops must be better!" Explain why this reasoning is not
logical when adding phenolphthalein indicator for an endpoint detennination.

*6. The mass of KHC8H404 is measured to the nearest milligram; however, the volume
of water in which it is dissolved is never of critical concern; water is even added to
the Erlenmeyer flask while washing the wall during the titration. Explain why the
addition of water to the Erlenmeyer flask is not critical to the analysis, whereas its
addition to the NaOH solution is critical.

38
EXPERIMENT 8 : ACIDS AND BASES ; PH

OBJECTIVES

To become familiar with the chemical and physical properties of acids and bases.
To measure the pH of laboratory and household acid, base, and salt solutions.

INTRODUCTION

Acids, both inorganic and organic, are important laboratory and industrial chemicals
primarily because, in aqueous solutions, they produce hydronium ions or because they are
oxidizing agents. Sulfuric acid is perhaps the most versatile of all inorganic industrial
chemicals. Presently, so many industries around the world use sulfuric acid that it is often
called the "old horse of chemistry." Chemically, a dilute solution of sulfuric acid acts as a
strong acid, providing hydronium ion to an aqueous system, whereas the concentrated
acid acts as a vigorous oxidizing agent and strong dehydrating agent. (Oxidizing agent: a
substance that removes electrons from another substance.) (Dehydrating agent: a
substance that absorbs water). Other inorganic acids of importance are hydrochloric acid,
nitric acid, and phosphoric acid. This experiment shows that hydrochloric acid is a
nonoxidizing acid, whereas nitric acid, like sulfuric acid, has excellent oxidizing properties.
Phosphoric acid is the additive in many soft drinks that deliver a tart taste. Some common
"organic" acids are acetic acid found in vinegar, citric acid found , in citrus fruits, and
ascorbic acid, the vitamin C. Other organic acids, such as formic acid, adipic acid,
terephthalic acid, oxalic acid, and oleic acid, are commercially useful and important. The
more familiar bases are aqueous ammonia (found in household Handy Andy ® and the
soluble metal hydroxides, sodium hydroxide (found in oven cleaner and drain cleaner),
called caustic soda or lye, calcium hydroxide, called slaked lime, magnesium hydroxide,
called milk of magnesia, and potassium hydroxide, called caustic potash. Other bases
used commercially are hydrated sodium carbonate, or soda ash or washing soda, used in
detergent formulations, and calcium oxide, or quicklime, used in cement.

ACIDIC SOLUTIONS

Acidic solutions have a sour taste, cause a pricking sensation on the skin, and tum blue
litmus (an acid-base indicator) red. Aqueous solutions become acidic because of the
presence of hydronium ions, H30 Acidic aqueous solutions result from the reaction of:

A nonmetallic hydride with water

Nonmetallic oxide with water

S03(g) + 2 H20(I) H30.,.(aq) + HS04-(aq)

C02(g) + 2 H20(1) H30.,.(aq) + HC03-(aq)

Molecular species with water

39
BASIC SOLUTIONS

A basic solution has a bitter taste, is slippery to the touch and turns red litmus blue.
Aqueous solutions become basic because of the presence of hydroxide ions, OW Most
household cleaning agents, such as soaps, detergents, and oven cleaners, are basic
solutions. The most common foodstuff that is basic is the wide collection of commercial
products called antacids. A basic solution can result from the action of :

Water on a soluble metallic oxide or hydroxide

NaOH(aq) Na"'(aq) + OH-(aq)

02-(aq, from, e.g., CaO) + H2O(1) 2 OH"(aq)

an anion that reacts with water

molecular species that react with water

In each case hydroxide ion is a product of the reaction. Other soluble carbonates, metallic
oxides, and substituted ammonia molecules behave similarly.

pH

The acidity or basicity of most aqueous solutions is frequently the result of low
concentrations of hydronium ion or hydroxide ion. To express these low concentrations
conveniently, PL. Sorensen, a Swedish chemist, introduced pH, the negative logarithm of
the molar concentration of hydronium ion.

Water dissociates very slightly, producing equal concentrations of hydronium ion and
hydroxide ion.

At 25°C, the molar concentration of hydronium ion, [H3O+], equals the molar concentration
of hydroxide ion, [OH1: both equal 1.0 X 10·7 mol/L. This results in a pH of 7. Addition of an
acid increases the [H3O•], causing a pH less than 7. A base decreases the (H30''] in
solution, producing a pH greater than 7. This experiment measures the pH of some acids
and bases. Acid-base indicators are generally organic compounds whose color depends
on the pH of the solution. Litmus is red in an acidic solution, but blue in a basic solution.
Mixtures of acid-base indicators can be used to approximate the pH of a solution. Various
pH test papers and universal indicator are examples of mixed indicators.

Ions of Salts as Acids and Bases

Salts ionize in aqueous solution to form cations and anions. Because of ion-dipole
interactions these ions are surrounded by polar water molecules (the ions are said to be
hydrated) to varying degrees. The If end of the water molecule is attracted to the cation of
the salt in solution and the ;+ end of the water molecule is attracted to the anion of the salt.

40
Generally the larger the charge and the smaller the size of the ion (charge and size are
collectively referred to as the charge density of the ion), the more strongly hydrated is the
ion. For example, the Fe3+ and A13+ cations are strongly hydrated because of their large
charge and small ionic size; the larger cations Ba2+ and cs• are only weakly hydrated. A
strongly hydrated cation, such as Fe3+,weakens the O-H bond of the hydrated water
molecule. This liberates H3O+ ion, producing an acidic solution. The pH of a solution
containing a cation with a large charge density is less than 7. A strongly hydrated anion,
such as PO/·, also weakens the O-H bond in water. But in this case OH· ion is liberated,
producing a basic solution. The pH of a solution containing an anion with a large charge
density is greater than 7. Cations and anions having a very weak attraction for water
molecules do not affect the pH of a solution. These ions typically have a low charge
density and are called spectator Ions with respect to pH effects. The common spectator
ions are cations: Group IA (Na+, "· Rb♦, Cs+), Group IIA (Mg2+, Ca2+, Sr2♦, Ba2+), and all
other metal cations having an oxidation number of 1+ anions: the halides (Cr, 8(, r), N03-
, C104-, and C103-.

EXPERIMENTAL PROCEDURE

Procedure Overview: The chemical properties of a range of acids and bases are
observed. The pH values of a range of acids and bases are estimated with pH test paper
or universal indicator. Included is the practice of following laboratory safety rules in
handling acids and bases. Combine your efforts and discuss your observations with a
partner. Caution: Dilute and concentrated (cone) acids and bases cause severe skin
burns and irritation to the mucous membrane. Be very careful in handling these chemicals.
Clean up all spills immediately with excess water, followed by a covering of baking soda,
NaHCO3. Refer to the Laboratory Safety section at the beginning of , this manual.

A. Acids and Acidic Solutions

1. Action of Acids on Metals. Put up a set of test tubes as follows: add 1ml into
labelled test tubes A1-A3 with 6M HCI, test tubes 81-B3 with 6M HNO3, and
test tubes C1-C3 with 6M CH3COOH. Polish with steel wool) small strips of Mg,
Zn, and Cu and place them as shown in the following table.

Mg Zn Cu
6MHCI A1 A2. A3
6M HNO3 81 B2 B3
6M CH3COOH C1 C2 C3

Observe closely for several minutes. Record your observations.

2. Effect of Acid Concentration on Reaction Rate. Add 1 ml into labelled test

tubes as follows.

D1 3M HCI
D2 0.1 M HCI
D3 0.01 M HCI
D4 3 M CH3COOH
D5 0:1 M CH3COOH
D6 0:01 M CH3COOH

41
 Add a polished 1-cm strip of Mg to each well and observe. Explain your obser-
vation. Account for any similarities and differences between CH3COOH and
HCI.

3. Oxidizing Strength of Acids. The iodide ion is readily oxidized to iodine with a
mild oxidizing agent. Place a few crystals (tip of a spatula) of Nal in labelled
test tubes A6 and B6. Add several drops of cone H2S04 (Careful!) to A6; to test
tube 86 add several drops of cone H3P04. What color changes, if any, do you
observe? Hold moistened blue litmus paper over each test well to test for any
escaping gases. What products form in these reactions? Disposal: Discard
the acid solutions in the 'Waste Acids" container. CLEANUP: Rinse the test
tubes twice with tap water and once with distilled water.

4. Dehydrating Effect of "Concentrated" Acids. (Caution: do not allow these

concentrated acids to touch the skin.) Test the dehydrating effects of cone
H2SO4 by placing a few drops on a wood splint and on a small amount of
sugar. Repeat the test with cone HCI. Record and explain your observations.

B. Bases and Basic Solutions

1. Reaction of Aqueous Sodium Hydroxide with Acid. Place about 1 ml of 1 M NaOH in

a 75-mm test tube. Test the solution with litmus. Add and count drops of 6 M HCl-
after each drop, swirl the mixture and test the solution with litmus-until the litmus
changes color.

2. Slaking of Quicklime. Place (about) 2 g of fresh, dry calcium oxide, CaO, in an

evaporating dish and add 1 ml of water (barely enough to moisten the quicklime). A
reaction, called slaking, should occur, with the generation of heat and the crumbling
of lumps. Write a balanced equation for the slaking of quicklime. Add additional
water until a thin paste forms. Test the solution with moistened litmus paper. A
saturated solution of calcium hydroxide is known as limewater. Disposal: Discard
the solutions from Parts B.1-B.2 in the "Waste Bases" container.

3. Production of Ammonia.

a. Set Up the Apparatus for the Collection of Ammonia. Set up the apparatus
shown in Figure 13.7. Place a mixture of 4 g (±0.01 g) of ammonium chloride,
NH4CI, and twice as much, by volume, of slaked lime into the 200-mm test
tube. Stir the mixture.

b. Generation and Collection of Ammonia. Heat the mixture gently; begin near
the mouth of the test tube and gradually extend the heating over the entire test
tube. As soon as gas evolves freely and the apparatus is free of air, collect four
bottles of ammonia gas by air displacement.( Consult your instructor on the
test for the presence of ammonia gas.) Cover each bottle with a glass plate or
stopper each bottle with a rubber stopper.

c. Test for the Flammability of Ammonia. Note the odour and colour of the NH3
gas. Test for its flammability by inserting a glowing wood splint into one of the
gas bottles. Consult your instructor on this technique.

42
 d. Test for the Solubility of Ammonia. Place about 300 ml of water in an 800ml
beaker. Add several drops of phenolphthalein to the water and stir. Submerge
the mouth of a bottle of ammonia beneath the water surface. Allow it to remain
there for 5 minutes; be sure the mouth of the bottle remains submerged. Note
the water level in the bottle and any color change of the water.

C. pH Measurements

Boil 10 ml of deionized water for about 10 minutes to expel any dissolved gases,
specifically carbon dioxide. Set the water aside to cool.

1. pH of Water. Put up a set of test tubes previously cleaned with soap and water
and rinse with deionized water. Add into test tubes labelled A1-A3 1ml boiled
(but cooled) deionized water, unboiled deionized water, and tap water,
respectively. Add 5 drops of universal indicator to each (color plate). Account
for any differences in the pH.

2. Estimate the pH of Acids and Bases. Place 1 ml of each solution listed on the
report sheet into test tubes 81-86 and add 5 drops of universal indicator to
each. Estimate the pH of each solution. Write an equation showing the origin of
the free H3O+or OH- in each solution.

3. Estimate the pH of "Common" Solutions. By the same method as in Part C.2,

use test tubes C1-C6 to determine the pH of vinegar, lemon juice, household
ammonia, detergent solution, Coca-cola®, Fanta®.

D. Ions of Salts as Acids and Bases

1. Estimate the pH of Each Solution. Transfer 1 ml of each solution listed on the

Bases Report Sheet into test tubes D1-D6 and add 5 drops of universal
indicator to each. Estimate the pH of each solution as in Part C. Identify the ion
that causes the acidity/basicity of the solution.

E. Acids and Bases

1. Neutralization of Acids. Put up a set of test tubes previously cleaned with soap
and water and rinsed with deionized water. Place 10 drops of 0.1 M HCI in test
tube A1, 10 drops of 0.1 M H2S04 in test tube A2, and 10 drops of 0.1 M
CH3COOH in test tube A3. Add 1 drop of phenolphthalein indicator to each test
tube. Add drops of 0.2 M NaOH to each test tube until a color change occurs
(swirl the solution after each drop). Record the drops added. Compare the
acidity of the three acids. Disposal and Cleanup: Discard the test solutions
into the sink. Rinse the with deionized water.

PRE-LABORATORY ASSIGNMENT

1. a. List some general properties of acids.

b. List some general properties of bases.

2. What is the color of the phenolphthalein indicator in a (a) basic solution? in (b) an
acidic solution?

43
3. Three solutions have the following pH:

Solution 1: pH 3.3
Solution 2: pH 9.7
Solution 3: pH 4.7

a. Which solution contains the highest H30+ion concentration?

b. Which solution is the most acidic?
c. Which solution is the most basic?

4. a. Which ion is more strongly hydrated, Fe3+ or Fe2+? Explain.

b. Which ion is more strongly hydrated, Li+ or K+? Explain.
c. Which of the following cations are not considered spectator ions with respect to
acid-base chemistry in an aqueous solution: Fe2+, Ca2+, K.., Cr+. and Cu2+?

5. Describe the chemical procedure for testing for the presence of NH3 gas in this
experiment.

6. a. What is limewater?
b. What is slaked lime?

REPORT SHEET

A. Acids and Acidic Solutions

1. Action of Acids on Metals. In the following table, state whether or not a reaction
is observed. Indicate the relative reactivity (i.e., fast, moderate, slow) of the
metals with the corresponding acid.

Mg Zn Cu
6MHCI
6 M HNO3
6 M CH3COOH

2. Effect of Acid Concentration on Reaction Rate.

a. Explain how changes in HCI concentration affect the reaction rate with Mg.

b. Explain how changes in CH3COOH concentration affect the reaction rate

with Mg.

c. Discuss the similarities and differences of HCI and CH3COOH in the

observed reactions with magnesium.

44