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EXPERIMENT 1

INTRODUCTION TO LABORATORY AND EXPERIMENTAL DATA

1.0 OBJECTIVES:
1.1 To introduce experimental data analysis using computer software.
1.2 To familiarize calculations, function equations, charting and graphing using Microsoft
Excel software.

2.0

INTRODUCTION:

2.1

Getting Started
Getting started with Excel 2007 you will notice that there are many similar features to
previous versions. You will also notice that there are many new features that youll be
able to utilize. There are three features that you should remember as you work within
Excel 2007: the Microsoft Office Button, the Quick Access Toolbar, and the Ribbon. The
function of these features will be more fully explored below.

2.1.1

Spreadsheets
A spreadsheet is an electronic document that stores various types of data. There are
vertical columns and horizontal rows. A cell is where the column and row intersect. A
cell can contain data and can be used in calculations of data within the spreadsheet.
An Excel spreadsheet can contain workbooks and worksheets. The workbook is the
holder for related worksheets.

2.1.2

Microsoft Office Button


The Microsoft Office Button performs many of the functions that were located in the
File menu of older versions of Excel. This button allows you to create a new workbook,
Open an existing workbook, save and save as, print, send, or close.

2.1.3

Ribbon
The ribbon is the panel at the top portion of the document It has seven tabs: Home,
Insert, Page Layouts, Formulas, Data, Review, and View. Each tab is divided into
groups. The groups are logical collections of features designed to perform function
that you will utilize in developing or editing your Excel spreadsheets.
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Commonly utilized features are displayed on the Ribbon. To view additional features
within each group, click the arrow at the bottom right corner of each group.

Home: Clipboard, Fonts, Alignment, Number, Styles, Cells, Editing.


Insert: Tables, Illustrations, Charts, Links, Text.
Page Layouts: Themes, Page Setup, Scale to Fit, Sheet Options, Arrange.
Formulas: Function Library, Defined Names, Formula Auditing, Calculation.
Data: Get External Data, Connections, Sort & Filter, Data Tools, Outline.
Review: Proofing, Comments, Changes.
View: Workbook Views, Show/Hide, Zoom, Window, Macros.

2.1.4

Quick Access Toolbar


The quick access toolbar is a customizable toolbar that contains commands that you
may want to use. You can place the quick access toolbar above or below the ribbon.
To change the location of the quick access toolbar, click on the arrow at the end of the
toolbar and click Show Below the Ribbon.

You can also add items to the quick access toolbar. Right click on any item in the
Office Button or the Ribbon and click Add to Quick Access Toolbar and a shortcut will
be added.

2.1.5

Mini Toolbar
A new feature in Office 2007 is the Mini Toolbar. This is a floating toolbar that is
displayed when you select text or right-click text. It displays common formatting tools,
such as Bold, Italics, Fonts, Font Size and Font Color.

2.2

Working with a Workbook

2.2.1

Create a Workbook
To create a new Workbook:
Click the Microsoft Office Toolbar.
Click New.
Choose Blank Document.

If you want to create a new document from a template, explore the templates and
choose one that fits your needs.

2.2.2

Save a Workbook
When you save a workbook, you have two choices: Save or Save As to save a
document:
Click the Microsoft Office Button.
Click Save.

You may need to use the Save As feature when you need to save a workbook under a
different name or to save it for earlier versions of Excel. Remember that older versions
of Excel will not be able to open an Excel 2007 worksheet unless you save it as an
Excel 97-2003 Format. To use the Save As feature:

2.2.3

Click the Microsoft Office Button


Click Save As
Type in the name for the Workbook
In the Save as Type box, choose Excel 97-2003 Workbook

Open a Workbook
To open an existing workbook:
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2.3

Click the Microsoft Office Button


Click Open
Browse to the workbook
Click the title of the workbook
Click Open

Entering Data
There are different ways to enter data in Excel: in an active cell or in the formula bar. To
enter data in an active cell:
Click in the cell where you want the data.
Begin typing.

To enter data into the formula bar


Click the cell where you would like the data.
Place the cursor in the Formula Bar.
Type in the data.

2.4

Charts
Charts allow you to present information contained in the worksheet in a graphic format.
Excel offers many types of charts including: Column, Line, Pie, Bar, Area, Scatter and
more. To view the charts available click the Insert Tab on the Ribbon.

2.4.1

Create a Chart
To create a chart:
Select the cells that contain the data you want to use in the chart.
Click the Insert tab on the Ribbon.
Click the type of Chart you want to create.

2.4.2

Modify a Chart
Once you have created a chart you can do several things to modify the chart. To move
the chart:

Click the Chart and Drag it another location on the same worksheet, or;
Click the Move Chart button on the Design tab.
Choose the desired location (either a new sheet or a current sheet in the
workbook).

To change the data included in the chart:

Click the Chart.


Click the Select Data button on the Design tab.

To reverse
which data
are displayed in the rows and columns:
Click the Chart.
Click the Switch Row/Column button on the Design tab.

To modify the labels and titles:


Click the Chart.
On the Layout tab, click the Chart Title or the Data Labels button.
Change the Title and click Enter.

2.4.3

Chart Tools

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The Chart Tools appear on the Ribbon when you click on the chart. The tools are
located
on
three
tabs:
Design,
Layout,
and
Format.
Within the Design tab you can control the chart type, layout, styles, and location.

Within the Layout tab you can control inserting pictures, shapes and text boxes, labels,
axes, background, and analysis.

Within the Format tab you can modify shape styles, word styles and size of the chart.

2.4.4

Copy a Chart to Word


Select the chart.
Click Copy on the Home tab.
Go to the Word document where you want the chart located.
Click Paste on the Home tab.

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2.5
2.5.1

Performing Calculations
Excel Formulas
A formula is a set of mathematical instructions that can be used in Excel to perform
calculations. Formals are started in the formula box with an = sign.

There are many elements to and excel formula.


References: The cell or range of cells that you want to use in your calculation.
Operators: Symbols (+, -, *, /, etc.) that specify the calculation to be performed.
Constants: Numbers or text values that do not change.
Functions: Predefined formulas in Excel
To create a basic formula in Excel:
Select the cell for the formula.
Type = (the equal sign) and the formula.
Click Enter.

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2.5.2

Calculate with Functions


A function is a built in formula in Excel. A function has a name and arguments (the
mathematical function) in parentheses. Common functions in Excel:
Sum: Adds all cells in the argument.
Average: Calculates the average of the cells in the argument.
Min: Finds the minimum value.
Max: Finds the maximum value.
Count: Finds the number of cells that contain a numerical value within a range of the
argument.
To calculate a function:
Click the cell where you want the function applied.
Click the Insert Function button.
Choose the function.
Click OK.

2.5.3

Complete the Number 1 box with the first cell in the range that you want
calculated.
Complete the Number 2 box with the last cell in the range that you want
calculated.

Relative, Absolute and Mixed References

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Calling cells by just their column and row labels (such as "A1") is called relative
referencing. When a formula contains relative referencing and it is copied from one
cell to another, Excel does not create an exact copy of the formula. It will change cell
addresses relative to the row and column they are moved to. For example, if a simple
addition formula in cell C1 "=(A1+B1)" is copied to cell C2, the formula would change to
"=(A2+B2)" to reflect the new row.
To prevent this change, cells must be called by absolute referencingand this is
accomplished by placing dollar signs "$" within the cell addresses in the formula.
Continuing the previous example, the formula in cell C1 would read "=($A$1+$B$1)" if
the value of cell C2 should be the sum of cells A1 and B1. Both the column and row of
both cells are absolute and will not change when copied.Mixed referencing can also
be used where only the row OR column fixed. For example, in the formula "=(A$1+
$B2)", the row of cell A1 is fixed and the column of cell B2 is fixed.
3.0 LABORATORY EXERCISE
3.1

Complete the data table by using Microsoft Excell 2007.


Volume,Ethanol
100
100
100
100
100
100
80
60
40
20
0

Volume,Water
0
20
40
60
80
100
100
100
100
100
100

Given;
Density of Ethanol
Density of Water
Molecular Mass of Ethanol
Molecular Mass of Water

No. of mole

3.2

Mole Fraction,Ethanol

Refractive Index
1.3650
1.3642
1.3630
1.3616
1.3602
1.3580
1.3552
1.3520
1.3474
1.3413
1.3336

= 0.79 g/cm3
= 1 g/cm3
= 46.041 g/mole
= 18 g/mole

= Density x Volume
Molecular Mass

Plot a graph of refractive index against mole fraction of ethanol.


In the graph, include the following information.
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3.3

3.2.1 Graph title.


3.2.2 Y and X axis title.
3.2.3 Trendline
3.2.4 Graph equation.
3.2.5 R square.
Print and make as a report
3.3.1
3.3.2

Copy the complete Excel table to Microsoft Word.


Copy the complete graph to Microsoft Word.

EXPERIMENT 2
MEASURE THE HEAT COMBUSTION OF AN ORGANIC SUBSTANCE
2.0

OBJECTIVES:
1.1
1.2

3.0

To determine heat combustion of organic substances.


To calculate the increasing temperature of organic substances.

INTRODUCTION :
In this experiment a bomb calorimeter is employed in the determination of the heat of
combustion of an organic substance such as naphthalene, C 10H8. The heat of combustion of
naphthalene is C10H8 for the reaction at constant temperature and pressure:
C10H8 (s) + 12O2 (g) = 10CO2 (g) + 4H2O(l)

4.0

(2.1)

THEORY:
Calorimetry is the science of measuring quantities of heat, as distinct from temperature. The
instruments used for such measurements are known as calorimeters. The most common type
of calorimeter is the oxygen bomb calorimeter. The Calorific Value of a sample may be broadly
defined as the number of heat units liberated by a unit mass of a sample when burned with
oxygen in an enclosure of constant volume. The calorific value as determined in an oxygen
bomb calorimeter is measured by a substitution procedure in which the heat obtained from the
sample is compared with the heat obtained from combustion of a similar amount of benzoic
acid whose calorific value is known. These measurements are obtained by burning a
representative sample in a high pressure oxygen atmosphere within a metal pressure vessel
called a bomb. The energy released by this combustion is absorbed within the calorimeter and
the resulting temperature change within the absorbing medium is noted. The calorific value of
the sample is then calculated by multiplying the temperature rise in the calorimeter by a
previously determined energy equivalent determined from previous tests with a standardizing
material.

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5.0

MATERIALS & EQUIPMENTS:


5.1
5.2
5.3
5.4
5.5
5.6
5.7
5.8
5.9

Calorimeter IKA C2000


Decomposition vessel (bomb)
Stainless steel crucible
Thermostatic bath can with compressed O2 pressure regulator
Analytical balance
Benzoic Acid
Unknown sample
Spatula
0.004-in. diameter iron wire (50 cm)

1) Control panel
2 )Keyboard
3 )Display
4 )Electronics unit
5 )Measuring cell
6 )Temperature sensor
7) Oxygen filling device
8) Decomposition vessel
(Accessory,please order seperately)
9)Measuring cell cover

Figure 2.1: Scheme of IKA C2000 calorimetric system.

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1) Cap screw.
2) Oxygen valve.
3) Cover.
4) Disposable crucible.
5) Electrical ignition contact.
6) Ignition wire.
7) Crucible holder.

Figure 2.2

Figure 2.3

Individual parts of the decomposition vessel.

Pressure reducer valve with manometers, mounted to pressure


gas can with O2.

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6.0

PROCEDURES:
6.1

Turning on the system:


a)

Check the connection of the gas can with oxygen, turn on the main valve and check
the oxygen pressure on the manometers.
b) Turn the chiller (thermostate) on and set up the working temperature as 20C. The
water level in the chiller must be in between maximum and minimum marks. If the
water less than minimum level, water must be added into the chiller by using 2 ml of
Aqua-Pro dilute with 1L distilled water.
c) Turn the calorimeter on.
6.2

Preparing the measurements:


a) Unscrew the cap screw and remove the cover by using the handle.

1) handle
2) cover
3) cap screw

Figure 2.4 Opening the decomposition vessel.

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b) Carefully open the decomposition vessel screw cap and install the ignite wire at the
electrical ignition contact (Refer Fig. 2.4). The ignite wire is very sensitive and
expensive. PLV will help you to install it.
c) Weight the empty disposable crucible and 0.50.1 g of benzoic acid. Slowly insert the
benzoic acid into the disposable crucible and place it at crucible holder. The sample
should be at the center of the wire. Handle it very carefully after weighing.
d) Carefully assemble the decomposition vessel and screw down the cap hand-tight;
never use a wrench.

e) Enter the weight of the combustion sample in the Weighed-in quant field. If an electric scale
is connected to the calorimeter system, the weight can be transferred automatically.
Depending on the type of scale, the Sample dialog box can be opened either by the sample
key of the calorimeter or with the Print/Transfer key of the scale. You can cause the scale
value to be accepted again by pressing the Space bar.
f) With Tab you can move the cursor to the following input fields. Fill up the space as follows:
i) QExtran 1 (use the following equation: )
QExtran1 = Gross calorific value of disposable crucible x weight of disposable crucible

ii) Sample name (automatically assign by the instrument)


iii) Sample proper (if there is any additional information)
iv) User (Name of user, minimum 8 characters)
v) Bomb and Cell (type 1 for each)
vi) [ ] Calibration (mark this field with the space bar if you want the system to use the
experiment for calibration)
With OK the system will accept input from the dialog box.

Note:
QExtran 1: Correction for the thermal energy from the cotton thread used as an ignition aid.
A preset value of 50 J/0 J (without/with combustible crucible) appears here. If you use a different
ignition aid instead of the IKAcotton thread, change this value as appropriate.
QExtran 2: Correction for the thermal energy from an additional combustion aid. The preset
value is 0. If the weight of the combustion aid is transferred in :With combustion aid mode from
electronic scale, the resulting extraneous energy calculated from the weight appears in the QExtran 2
box.
Even without a scale, the gross calorific value of the combustion aid can be taken into consideration
automatically. In this case, you should enter the weighed in quantity of the combustion aid in the
QExtran 2 box and then press the arrow down. QExtran 2 is calculated according to the formula
QExtran 2 = Weighed in quantity of combustion aid x calorific value of combustion aid

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and is entered in the QExtran 2 box. If a value > 10 J is entered, it is assumed that the value already
represents all extraneous energy QExtran 2 In this case, there is no further conversion based on the
formula given above.

6.3

Preparing the measurements:


a) Guide the decomposition vessel into the filler head of the open measuring cell cover until it
catches in place. The decomposition vessel maintains a defined position in the holder on the fill
head by being lowered at the center of the fill head by 0.8 mm. A spring element then makes
contact with the electrical ignition contact on the decomposition vessel (Refer Fig 2.5 ).
b) The message "Bomb securely closed?" will appear. Ensure that the decomposition vessel is
properly closed and confirm with OK.
The ignition wire in the decomposition vessel completes the electrical circuit. The calorimeter is
ready to start. The message Bomb changes to a display of the function key assignment Start.
If the Start function key does not appear, please check the ignition wire of the decomposition
vessel.

1
2
3
4

Figure 2.5

cap screw
filling head
ignition contact
spring element

Suspending the decomposition vessel into the filler head of the measuring cylinder.

c) Push the Start button.


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d) After this the measuring cell cover closes. The decomposition vessel is filled with oxygen (for
about 60 sec.). After the temperature in the outer vessel has stabilized
(90 -120 sec.), the
inner vessel fills with water. As soon as the system starts the experiment, the display shows the
course of the temperature of the inner vessel over time as a graph .

The measurement proceeds fully automatically until the final result. Write down the gross calorific value
or C value that was determined during experiment.
7.0

RESULTS:
1.

Weight of empty disposable crucible (g) :


Gross calorific of disposable crucible (g):
Gross calorific of your sample (g) :
a) Benzoic acid
b) Sample A
c) Sample B
d) Sample C

2. Determine the increase of temperature Tcal for each sample including correction factor
according to these equations:

Where:
Tn last value of temperature in the main period,
To - last value of temperature in the initial period

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c correction for heat exchange between calorimeter


and surrounding.
Correcting factor c is calculated by Buntes formula:

where:
nt - number of temperature points recorded per minute
i - mean value of temperature increase (in K or C) per one minute during the initial period
f - a mean value of temperature decrease (in K or C) per one minute during the final period
r - number of temperature points recorded during the main period.

8.0

9.0

DISCUSSIONS:
8.1

Find the literature value for your sample and compare it to the value you obtained. If
the results are different then discussing why this is so.

8.2

Discuss the magnitude of the uncertainty introduced by lack of knowledge of the


specific heat of the sample? Does your H value pertain to the initial or the final
temperature?

CONCLUSIONS:
9.1

Based on the experimental procedure done and the results taken, write the
conclusion to this experiment.

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EXPERIMENT 3
DETERMINE OF THERMODYNAMIC OF ICE CREAM MIXTURE
1.0

OBJECTIVES:
1.1
1.2

2.0

To determine the freezing point of ice cream mixture.


To evaluate the heat/energy did the ice cream mixture need to turn it to a solid.

INTRODUCTION:
Its about 35oC in the shade and to cool off, you are eating an ice cream cone. As you sit
there, you wonder just how ice cream is made. One area of chemistry that helps explain the
making of ice cream is thermodynamics. There are three laws of thermodynamics:
1. The total amount of energy in the universe is constant.
2. The entropy of the universe is always increasing.
3. Everything with a temperature above zero Kelvins has energy.

3.0

THEORY:
You may recognize the first law of thermodynamics as the law of conservation of energy. The
second law may be more familiar to you when it is expressed in everyday language: heat
always flows from a warmer object to a cooler object. In making ice cream, it is this
second law that is of interest.
Another aspect of chemistry involved in producing ice cream deals with the physical properties
of solutions, which differ from those of pure solvents. In the presence of solute particles in a
solution will raise the boiling point or lower the freezing point of the solvent, depending of the
number of particles dissolved in a given mass of solvent. The latter characteristics apply to
ice cream because the ice cream mixture is mainly a solution of sugar in water, and its freezing
point is depressed below 0oC.

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Before refrigerators were invented ice cream was made using ice. In order to solidify by this
method, the hot ice cream mixture has to lose energy to the cold ice. Since ordinary ice is
only at 0oC, however, the lowest temperature that the ice cream mixture can reach is 0 oC.
With the system at thermal equilibrium (the ice cream and the ice are at the same
temperature), the ice cream would still be a liquid.

To freeze the ice cream mixture, it is necessary to use colder ice. How do you do that?
Again, what you know about colligative properties provides the answer: you make a solution.
A salt-ice mixture has a lower freezing point than pure ice, so it acts as colder ice. The
more salt added to the ice, the lower the freezing point. The ice cream mixture can lose
more energy to the salt-ice mixture and freeze before thermal equilibrium is reached.

4.0

MATERIALS & EQUIPMENTS:


4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8

4 oz baby food jar with lid


Ice cream mixture
Coffee can with lids
Crush ice
Rock salt
Thermometer
Cloth towel
Spatula/spoon

5.0 PROCEDURES:
5.1
5.2

5.3

5.4

Describe the ice cream mixture before you begin and record your observation in the
Data Table 3.1.
Use a spatula/spoon to fill a clean baby-food jar three-fourth of the way with the ice
cream mixture. Seal the jar tightly with the lid. (If the jar leak, the ice cream will be
salty).
Use another spatula/spoon to fill a large can about one third full with half of the ice
and half width of the rock salt. Describe the salt-ice mixture. Measure and record its
temperature.
Put the closed baby jar in the can and surround it with the rest of the ice and the salt.
Put the lid on the can (Fig. 3.1).

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Figure 3.1: The salt-ice


mixture setup
5.5 Wrap the can in a towel to insulate it and to protect your hands.
Roll the can back
and forth on the table, countertop or floor for
about 15 minutes. Unwrap the can
and describe it.
5.6 Take the lid of the can and describe the salt- ice mixture.
Measure and record the
temperature of the salt ice mixture. Remove and rinse the baby food jar, open the cap,
and wipe the rim free of salt.
5.7 Describe the appearance of the ice cream mixture. Test the product.
5.8 Wash the jar, can, lids and spatula/spoon. Pour the salt-ice mixture down to the drain with
plenty of water. Clean up work station and wash your hands before leaving
the
laboratory.
6.0

RESULTS:
6.1

Write the initial and final salt-ice temperature as in Table 1 below:

Salt-Ice Temperature:

Table 3.1: Data Chart


Initially:

Finally:

______oC

Describe the physical look of the ice mixture


Initially:

Observation:

Initially:

Finally

Describe the can look after it is rolled


Finally

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6.2
6.3
6.4

6.5

7.0

Calculate the theoretical freezing point depression of the ice-salt mixture used in this
experiment.
Compare your actual freezing point to the one calculated. Determine the percent error.
Identify the final temperature of the water and calculate how much heat does the water
absorb (Use 1150 g for the mass of the mixture, and use 4.18 J/g oC as the specific
heat for the water).
Evaluate how much heat/energy did the ice cream mixture needs to turn it to a solid.

DISCUSSIONS:
7.1
7.2
7.3

8.0

Explain the ice cream system either exothermic or endothermic reaction.


Explain how could you have speed up the freezing of the ice cream mixture.
Using the concepts learned in the lab, and your knowledge, why do people put salt
on their sidewalks in the winter time.

CONCLUSION:
8.1

Based on the experimental procedure done and the results taken, write the conclusion
to this experiment.

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EXPERIMENT 4
DETERMINATION OF CHEMICAL EQUILIBRIUM

1.0

OBJECTIVES:
1.1
1.2

2.0

To determine the chemical equilibrium for the reaction.


To calculate the equilibrium constant for the reaction.

INTRODUCTION:
Many chemical reactions, especially those of organic substances, do not go to completion.
Rather, they come to a point of chemical equilibrium before the reactants are fully converted
to products. At the point of equilibrium, the concentrations of all reactants remain constant with
time. The position of equilibrium is described by a function called the equilibrium constant,
Kc, which is the ratio of the amount of product present to the amount of reactant remaining
once the point of equilibrium has been reached. You will determine the equilibrium constant for
an esterification reaction.
Early in the study of chemical reactions, it was noted that many chemical reactions do not
produce as much product as might be expected, based on the amounts of reactants taken
originally. Somewhat like why the batch of cookie dough never yields the number of cookies
the recipe promises?
Some reactions appear to stop because the products produced by the original reaction
themselves begin to react, in the reverse direction to the original process. As the concentration
of products begins to build up, product molecules will react more and more frequently.
Eventually, as the speed of the forward reaction decreases while the speed of the reverse
reaction increases, the forward and reverse processes will be going on at exactly the same
rate. Once the forward and reverse rates of reaction are identical, there can be no further net
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change in the concentrations of any of the species in the system. At this point, a dynamic state
of equilibrium has been reached. The original reaction is still taking place but is opposed by
the reverse of the original reaction also taking place.
3.0

THEORY:
In this experiment you will determine the equilibrium constant for the esterification reaction
between n-propyl alcohol and acetic acid which forms n-propyl acetate (an ester) and water:
CH3CHOOH

+CH3CH2CH2OH CH3COOCH2CH2CH3

+ H2O

You will set up the reaction is such a way that the initial concentrations of the reactants are
known. The reaction will then be allowed to stand for one week to come to equilibrium. As the
reactants react the acidity of the mixture will decrease, reaching a minimum once the system
reaches equilibrium. You will be able to qualitatively be able to measure this with your sense of
smell. Week one the acetic acid is strong (vinegar) and week two it will smell like the ester npropyl acetate which is a common component of nail polish remover.
The quantity of acid present in the system will be determined by titration with a standard
sodium hydroxide solution. Esterification reactions are typically catalyzed by the addition of a
strong mineral acid. You will be using a small amount of 6M sulfuric acid as a catalyst. The
concentration of acetic acid in the mixture is determined by the technique of titration. Acetic
acid reacts with sodium hydroxide on a 1:1 stoichiometric basis.
4.0

MATERIALS & EQUIPMENTS:


4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8

5.0

50 mL buret
Plastic wrap
Standard 0.1 M NaOH solution
Phenolphthalein indicator solution
1 mL pipet and pump
1-propanol
Acetic acid glacial
6 M Sulfuric acid

PROCEDURES:
Week 1: Four total titrations need to be complete before it sits for a week
5.1

Obtain approximately 100 mL of standard 0.10 M NaOH solution in a clean, dry


beaker.

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5.2

5.3

5.4

5.5
5.6

5.7

5.8

Rinse the buret several times with small portions of NaOH solution (discard the
rinsings), then fill the buret with NaOH solution. Keep the remainder of the NaOH
solution in the beaker covered until it is needed.
Clean two 250 mL Erlenmeyer flasks for use as titration vessels. Rinse the flasks with
tap water; follow with small portions of distilled water. Place approximately 25 mL of
distilled water in each flask, and set aside until needed.
Clean and dry a 125 mL Erlenmeyer flask. Label the flask as reaction mixture.
Cover a rubber stopper with plastic wrap or baggie. This will contain the mixture for
the entire lab and will need to be used next week. Rubber stoppers will be
decomposed by the vapors of the reaction mixture unless there is plastic protection.
Clean and dry a small graduated cylinder. Using the graduate, obtain 14 0.2 mL of
glacial acetic acid (0.25 mol) and transfer the acetic acid to the reaction mixture flask.
Rinse the graduated cylinder with water and re-dry. Obtain
19 0.2 mL of 1propanol (0.25 mol) and add to the acetic acid in the reaction mixture flask. Stopper
the flask and swirl the flask for several minutes to mix the reagents.
By using the 1 mL pipet, transfer 1.00 mL of the reaction mixture to each of the two
250 mL Erlenmeyer flasks. Re-stopper the flask containing the reaction mixture to
prevent evaporation. Add 3-4 drops of phenolphthalein indicator to each of the two
samples to be titrated.
Titrate each mixture until the pale light permanent pink color appears. Be sure to pay
attention to the level of NaOH in the buret and do not let it run below the 50 mL mark.
Refill as necessary keeping a record of total volume added during the titration. Record
the amount of NaOH added for each trial. Discard the two trials.

Adding and analyzing catalyst:


5.9
5.10

5.11

**Do not add catalyst unless you have time to do the last two titrations. Be sure to complete
them today so the reaction mixture can sit for a complete week until the next lab session.
Refill buret (if needed) with standard solution NaOH. Clean out the titration flasks, rinse, and fill
with approximately 25 mL of distilled water. Add, with swirling, 10 drops of 6 M sulfuric acid
catalyst to the reaction mixture. Immediately pipet a 1.00 mL sample of the catalyzed
reaction mixture into each of the titration flasks. Do not delay pipetting, or the concentration of
acetic acid will begin to change as the reaction occurs.
Titrate these two samples with the NaOH, record volume used for trials 3 & 4. Stopper the 125
mL flask containing the acetic acid/1-propanol mixture. Place the reaction mixture in your
locker until next week.

Week 2: Only two titration trials needed


5.12
5.13

After standing for a week, the reaction system of 1-propanol and acetic acid will have come to
equilibrium.
Rinse a buret and 1 mL pipet with distilled water. Rinse and fill buret with the standard 0.10 M
NaOH solution.
29

5.14

5.16

Clean and rinse two 250 mL Erlenmeyer flasks. Place approximately 25 mL of distilled water in
each of the flasks. Uncover your reaction mixture. Pipet 1 mL samples into each of the two
flasks. You should notice the odor of the reaction mixture has changed markedly from the
sharp vinegar odor of acetic acid that was present last week.
Add 3-4 drops of phenolphthalein to each sample, and titrate the samples to the pale pink
endpoint with the standard NaOH solution; record the total volume added in each flask.
Complete the data in Table 4.1 and done the calculations.

6. 0

RESULTS:

6.1

Complete the following table:

5.15

Table 4.1: Data table for the titration.


WEEK ONE

Trial 1
uncatalyzed

Trial 2
uncatalyzed

Trial 5

Trial 6

Trial 3
catalyzed

Trial 4 catalyzed

Initial buret volume


Final buret volume
Total volume NaOH
used
WEEK TWO
Initial buret volume
Final buret volume
Total volume NaOH
used
6.2

Concentration of standard NaOH solution________.


Table 4.2: Data table for the concentration of each sample.

a. Volume of NaOH to titrate 1 mL initial Trial 1


uncatalyzed mixture (1st week)
Mean volume
30

Trial 2

b. Concentration of acetic acid, M, in


original mixture
c. Volume of NaOH to titrate 1 mL Trial 3
catalyzed reaction mixture (1st week)

Trial 4

Mean volume
d. Volume correction for sulfuric acid
e. Volume of NaOH to titrate 1 mL of Trial 5
equilibrium mixture (2nd week)

Trial 6

Mean volume
f. Volume (corrected) of NaOH to titrate
acetic acid in equilibrium mixture
g. Concentration of acetic acid, M, in
equilibrium mixture
h. Change in concentration of acetic acid
in reaching equilibrium
6.3

Determine the chemical equilibrium of this reaction.

6.4

Complete ICE box using the information above:

I
C
E

Calculate the equilibrium constant for the reaction. Using the theoretical value for this reaction and
calculate the percent error.
7.0

DISCUSSIONS:
7.1

7.2

Sulfuric acid was used as a catalyst in this reaction. Would the presence of a catalyst
affect the position of the equilibrium (the relative amounts of substances present once
equilibrium was reached)? Explain why?
Could some other acid have been used as the catalyst? Explain Why?

31

7.3

7.4

7.5

8.0

The 6 M sulfuric acid used as the catalyst for this reaction quite naturally contains
some water, and water is one of the products of the esterification reaction. Explain how
will the presence of a small amount of water in the catalyst affect the position of the
acetic acid/1-propanol equilibrium? Discuss how will this water affect the value
determined for the equilibrium constant?
A common misconception among students is that you leave liquids and solids out of
equilibrium constants. All the species involved in this reaction were liquids, and all of
their concentrations were included in the calculation of the equilibrium constant.
Explain in your own words.
How would a change in temperature affect the equilibrium reaction studied? (Assume it
is exothermic) Would the position of equilibrium change? Would the value of the
equilibrium constant change? Explain in your own words.

CONCLUSION:
8.1

Based on the experimental procedure done and the results taken, write the conclusion
to this experiment.

32

EXPERIMENT 5
DETERMINE THE KINETICS OF THE REDUCTION OF METHYLENE BLUE
1.0

OBJECTIVES:
1.1
1.2

2.0

To illustrate the spectra of methylene blue solution.


To calculate the kinetic rate of the reduction of methylene blue.
INTRODUCTION:

Chemical kinetics is the study of properties of chemical processes such as reaction rates,
mechanisms and transition
states. The mechanism and rate of chemical reactions can be
determined using UV-Visible spectrophotometry.
Methylene blue (MB+) is a water-soluble dye molecule. Under acidic conditions, it is easily
reduced to the colorless hydrogenated molecule leucomethylene blue (LB +) by ascorbic acid
(H2A) as shown in Figure 5.1. The stoichiometry of the overall reaction is 1:1 and is
represented in the equation:
MB+ + H2A LB+ + D

Methylene Blue (MB+), blue color


Ascorbic Acid (H2A)

Leucomethylene Blue (LB+), colorless


33

Dehydroascorbic Acid (D)

Figure 5.1: Reaction mechanism of methylene blue with ascorbic acid.

3.0

THEORY:
Understanding a chemical reaction requires one to determine the mechanism of reaction,
predict it by some plausible set of elementary steps, determine the rate constants involved,
and predict the magnitudes of the various parameters, if possible. Mechanisms can be
quite involved, as for example in the catalyzed decomposition of ozone or the formation of
HCl fromH2 and Cl2, even though the overall reaction may appear simple. Consider the
simplest single-step mechanisms. For example, one is the transformation of a reactant A to
product, which is of first order at all times:
A Product

(5.1)

For such a first-order reaction, the rate equation is:

(5.2)
where CA is the reactant concentration and k1 is the first-order rate constant. The solution
of this equation gives the manner in which the concentration of reactant changes with time:
(5.3)

This is the linearized form of the rate equation. A plot of the logarithm of the concentration
versus t is a straight line, with a slope of k1. From the slope of such a plot, one extracts the
rate constant.
Some reactions do not go to completion as assumed in the previous paragraph. In the
following two-step mechanism, A converts to B, and B is converted to A, both by first-order
processes.

(5.4)
The equation for the

disappearance of A by this mechanism is:


34

(5.5)

The equation for the rate of appearance of B is identical in form. The solution of this equation
is:
(5.6)

where the concentration at any time t is given by CA(t). In particular, after a very long time
(indicated by ), the reaction may produce a state in which both A and B are present.
For this mechanism, the linearized form of the equation is also logarithmic, however the
argument of the logarithm is a difference of
concentrations, so one has to form a function
of concentrations to
determine the rate constants, but these are available from the
measured concentrations of A. The situation is shown in Fig. 5.2.

Figure 5.2: First-order approach to equilibrium. The lines on the left indicate the equilibrium
values of the concentration of the two components.
This mechanism illustrates the approach to dynamic equilibrium. It appears from equation (5.6)
that the only information from such a graph is the sum of the rate constants. However, at
dynamic equilibrium (i.e. at very long times), the rates of these two processes are equal,
which allows one to determine the ratio of the rate constants.
35

(5.7)

From this equation and the slope of an appropriate logarithmic graph, one has two
equations in
two unknowns, which allows an independent evaluation of both k1 and k-1.
Dynamic equilibrium
is very important. Consider, for example, a reaction sequence in which the
forward step is of first order in A and the reverse step is of second order in B. While the
mathematics of the
solution of the equation at any time may be
difficult, at equilibrium the
two rates must be
equal, which gives a
relationship between the two rates constants and the
equilibrium
concentrations:
(5.2)

in which the rate constant of the reverse step, since it is of second

order, is labeled k2.

Second-order reactions form an important class in kinetics. There are two kinds of secondorder reaction steps, those that are of second order in a single species, and those that are of
second order by virtue of being first-order in each of two distinguishable species. Consider
the simplest second-order mechanism that this just a single step of the former type. The
reaction is:
2 A Product

(5.9)

and the velocity equation is:


(5.10)

The solution of this equation gives the time course of the reactant:
(5.11)

This is the linearized form of the equation, so a plot of the inverse of the concentration of a
reactant versus time should give a straight line, the slope of which is 2k2.
The second form occurs for reaction of two distinguishable species (each having a unique
starting concentration) that react in a one-to-one step to form products:
A + B Product
36

(5.12)

The rate equation derivable for this process is:


(5.13)

This differential equation may be solved, subject to known initial concentrations, to give the
following complex equation:
(5.14)
The function that one must plot to obtain a linearized form of the rate
law requires one to
measure simultaneously and independently the concentrations of both reactants. If that can
be done, a plot of the logarithm of the ratios of the concentrations gives a straight line with a
slope of (CB(0)-CA(0))k2, from which one may extract the rate constant.
The form of the equation (5.14) becomes indeterminate for the condition that the initial
concentrations of the two species are equal. One may show that, under these conditions, one
need only follow the concentration of one species (since the other must always be of identical
concentration). The equation for its change is similar to that of
the identical-species second
order result:
(5.15)
Except that the slope is the rate constant for the reaction. This is obviously mathematically
simpler to analyze than equation (7.14), but the difficulty of ensuring that the initial
concentrations of the two reactants are identical provides a practical barrier to using this
technique.
Limiting Reagents
Consider the situation in which a reaction of the type in equation (5.12) is carried out under
conditions that one reagent is present at concentrations many hundreds or thousands of times
lower than the concentration of any other. Under these conditions, even though the
concentration of the reagent in excess is changing, the changes are so slight that it may be
considered, practically, constant over the course of the experiment. Then, to a very good order
of approximation, the rate equation for a process that obeys equation (5.12) is:
(5.16)
where
(5.17)
37

if A is the material present in limited amounts. Equation (5.16) is of the same form as equation
(5.2). The solution is of the same form:
(5.18)
Under these conditions in which A is a limiting reagent, one may follow the concentration of the
limiting reagent to determine the effective rate constant.
The idea of limiting reagents is much more general than just first-order reaction steps.
For example, consider the reaction:
A + B nb Product

(5.19)

which is not necessarily an elementary reaction, but denotes the relative stoichiometry. Then
one may write a general rate equation for the loss of A.
(5.20)
where m and n are the orders with respect to A and B, respectively. Under the condition that B
is present in large excess, this equation simplifies to:
(5.21)
where
(5.22)
For example, m = 1 gives equation (5.18), but if m = 2, this technique gives a second-order
dependence of CA on time, and so forth. The use of limiting reagents gives a means to
determine the effective rate constant from a plot, provided one can measure the concentration
of the limiting reagent as a function of time.
Equation (5.22) also indicates another feature of the use of a limiting reagent. A series of
studies of the effective rate constant for a reaction in which the excess reagents concentration
is changed (but still remains in excess) gives a means of determining the order with respect to
that reagent as well. Equation (5.22) may be rewritten in the form:
(5.23)

38

A plot of the logarithm of the effective rate constant versus the logarithm of the concentration of
the excess reagent is a straight line with a slope that gives the order and an intercept that is
the logarithm of the rate constant.

4.0
4.2
4.3
4.4
4.5
4.6
4.7

MATERIALS & EQUIPMENTS:


4.1 0.0004 M Methylene blue
0.1 M Ascorbic Acid
1.2 M Hydrochloric Acid (HCl)
Distilled water
Dioinized water
10 mL Volumetric flask
Pipette
5.0 PROCEDURES:

5.1

5.2

5.3

5.4
5.5

5.6

5.7

You need several solutions. Make a stock solution of 50 mL of methylene blue in distilled
water at an approximate concentration of 0.0004 M and approximately 50 mL of an ascorbic
acid in distilled water at approximately 0.1 M. There should be a stock solution of HCl available
in the laboratory.
From these, you make a series of solutions, so it is important
that you make the
solutions carefully and know the concentrations precisely. There are three sets of experiments
you must run.
In the first set of kinetics experiments (called the A set), you
hold
the
HCl
concentration in the solution constant at some value near 0.06 M usually a concentration
near that of the stock solution) and the ascorbic acid concentration constant at some value
near 0.025 M. (In advance, you must calculate how much of the stock solutions to add to
ensure that the final concentration is an appropriate value.)
Make up these solutions using 10 mL volumetric flasks, always adding the methylene blue
last, mixing, and quickly add the material to the cuvette.
In this set of experiments, the concentration of methylene blue
should be varied
-6
over several concentrations that span the range from about 5x10 to about 4x10-5 M.
(Important: add the methylene blue component immediately before you are ready to begin
the experiment, and add water to volume.)
In the second set of kinetics experiments (called the B set),
you should fix the
concentrations of HCl (at some concentration around 0.06 M) and the methylene blue (at some
concentration near 1.5x10-5 M), and vary the ascorbic-acid concentration (from 0 up to about
0.04 M). Again, add
the methylene blue last immediately before running the kinetics run.
In the third set of kinetics experiments (called the C set), fix
the ascorbic acid
concentration at some value near 0.04 M and the methylene blue concentration at the
concentration of 1.5x10-5 M of the previous runs. In this set, vary the HCl concentration from
0.01 to about 0.06 M.
39

5.8

The easiest way to create solutions is to determine how much


of
the
stock
solutions of HCl, ascorbic acid, and methylene blue must be added to the 10-mL volumetric
flask for each solution. Add the HCl and ascorbic acid.
When you are ready to start a run, quickly add the proper volume of methylene blue
solution, mix and pipette to the cuvette, turn the cuvette once or twice to mix the materials,
insert in the UV spectrophotometer and immediately begin taking data with the kinetics
program.
To do this, you must have determined beforehand how much of each of the stock
solutions you are to add to the cuvette to produce the appropriate concentrations and have the
spectrophotometer ready to go. It is extremely important that you clean the cuvettes and
glassware thoroughly between runs and before starting the experiments. Rinse all glassware
including cuvettes with 0.1 M HCl and then rinse them with copious amount of deionized water
several times before use. If you do this, you should get very good, reproducible data.

5.9

5.10

6.0 RESULTS:
6.1

6.2

6.3

6.4

7.0

Plot the spectra of methylene blue solution and the solution of


final products from
200 to 800 nm. The most convenient means to do this is with a program such as
EXCEL. After bringing the data into EXCEL, you will have a set of x and y data.
Analyze each set of kinetic data with a program like EXCEL. As in calculation 1, you
have to generate x data. Before analysis, be sure to find the long-time absorption and
subtract this from each point, so that you are looking at only the time-varying part of
the absorption. For part A, analyze each kinetics run as first order or second order in
methylene blue. After this part, you should decide whether this reaction is most
appropriately considered a first-order or a second order reaction in methylene blue.
In subsequent analyses, use this information and only analyze the data in the manner
you decide the data are changing.
For the data in part B, extract the effective rate constant for each of the runs from an
appropriate plot. This rate constant depends on the ascorbic concentration. Since
methyleneblue is a limiting reagent, one may use equation (5.23) to determine the
order with respect to ascorbic acid from a plot of the effective rate constant versus
ascorbic acid concentration.
For the data of part C, do a similar analysis as in calculation 3 to determine the order
with respect to hydrochloric acid.
DISCUSSIONS:

7.1
7.2
7.3

Based on these analyses, is the order with respect to methylene blue first or
second?Explain evidence do you have for this finding?
Discuss what are the orders with respect to ascorbic acid and hydrochloric acid?
Write the rate law for this reaction as you know it from your experiments.

40

8.0

CONCLUSION:
8.1 Based on the experimental procedure done and the results taken, write the conclusion
to this experiment.

41

EXPERIMENT 6
DETERMINE THE KINETIC HYDROLYSIS OF ETHYL ACETATE
1.0

OBJECTIVES:
1.1
1.2

2.0

To determine the rate constants and the activation energy of the alkaline hydrolysis of
ethyl acetate using sodium hydroxide.
To evaluate the rate order of the reaction.

INTRODUCTIONS:
Chemical kinetics is the part of physical chemistry that study reaction rates. The reaction rate
or rate of reaction for a reactant or product in a particular reaction is intuitively defined as how
fast a reaction takes place. For an example The hydrolysis of an ester (ethyl acetate) in
acidic solution will be studied for different temperatures. For each temperature, the progress of
the reaction will be tracked by pH measurements after certain time steps, which will in turn
yield the reaction rates.

3.0 THEORY:
Consider a typical chemical reaction:
aA + bB pP + Qq

(6.1)

The lowercase letters (a, b, p, and q) represent stoichiometri coefficients, while the capital
letters represent the reactants (A and B) and the products (P and Q).
According to IUPAC's Gold Book definition the reaction rate v for a
chemical reaction
occurring in a closed system under constant-volume
conditions, without a build-up of
reaction intermediates, is
defined as:

(6.2)

Where cI, I=A, B, P, or Q is the concentration of substance. The IUPAC recommends that the
unit of time should always be the second. Reaction rate usually has the units of mol dm-3 s-1.
It is important to bear in mind that the previous definition is only valid for a single reaction, in a
closed system of constant volume.

42

The quantity:
(6.3)

Defined by the equation


(6.4)
where nI designates the amount of
substance I (I=A, B, P, or Q)
conventionally expressed in
units of mole, may be called the 'rate
of
conversion' (extent of reaction) and is appropriate
when the use of concentrations is
inconvenient, e.g. under conditions of varying
volume. In a
system of constant volume, the rate
of reaction is equal to the rate of conversion per unit
volume throughout the reaction. For a
stepwise reaction this definition of 'rate of reaction'
(and 'extent of reaction', x) will
apply only if there is no accumulation of intermediate or formation of side products. It is therefore
recommended that the term 'rate of reaction' be
used only in cases where it is experimentally
established that these conditions apply. The rate law or rate equation for a chemical reaction is an
equation which links the reaction rate
with concentrations or pressures of reactants and constant
parameters
(normally rate coefficients and partial reaction orders). To determine
the
rate
equation for a particular system one combines the reaction rate with a mass balance for the system.
For a generic reaction A + B C the simple rate equation is of the form:
(6.5)
the concentration is usually in mol/dm3, and k is known as the reaction rate coefficient or
rate constant, although it is not really a constant, because it includes everything that affects
reaction rate outside concentration: mainly temperature but also ionic strength, surface
area of the adsorbent or light irradiation. The exponents n and m are called reaction
orders and depend on the reaction mechanism. The
stoichiometric coefficients and
reaction orders are very often equal, but only in one step reactions, molecularity (number of
molecules or atoms actually colliding), stoichiometry and reaction order must be the
same.
Since many complex reactions proceed in stages via intermediates (eg. ions, molecules or free
radicals), and, since the measured rate is always that of the slowest step, a knowledge of the
overall order, or better, the separate orders with respect to the individual reactants,
often enables the steps to be elucidated. In such circumstances, the rate of reaction cannot
be expressed as a simple equation.

43

The Arrhenius equation is a simple, but remarkably accurate, formula for the temperature
dependence of the rate constant, and therefore rate, of a chemical reaction. Actually, the
Arrhenius equation gives "the dependence of the rate constant k of chemical reactions on the
temperature T (in Kelvin) and activation energy Ea", as shown below:
(6.6)
where A is the pre-exponential factor or simply the prefactor and R is the gas constant.
The
units of the pre-exponential factor are identical to those of the rate constant and will vary
depending on the order of the reaction. It can be seen that either increasing the temperature or
decreasing the activation energy (for example through the use of catalysts) will result in an
increase in rate of reaction. The activation energy can be interpreted as the minimal energy of
the molecules to undergo reaction. This energy is needed, either, to rupture a chemical
bond, eg. in free radical gas reactions, or to allow rearrangements when the molecules collide.
Taking the natural logarithm of the Arrhenius equation yields:
(6.7)

So, when a reaction has a rate constant which obeys the Arrhenius equation, a plot of ln k
versus T -1 gives a straight line, whose slope and intercept can be used to determine Ea and
A. This procedure has become common in experimental chemical kinetics. To determine the
activation energy of a reaction, one must know a rate constant of the reaction at least at two
different temperatures. Applying the Eq. 6, one can easy express

(6.8)
where k1 and k2 correspond to temperature T1 and T2, respectively.
Since the rate of a given reaction depends upon the concentration of
the reactants, the
speed of the process falls off as the reaction
proceeds, for the reactants being
continuously consumed. The
reaction is becoming slower and slower but theoretically
never ceases. It is, therefore, not possible to define the general rate of a reaction,
and
so in practice the rate is considered at a particular instant. The rate may be defined in any
convenient way, usually, the rate of
change of concentration (c) of one of the reactants or
products is
chosen. The experimental data then follow a change of concentration
with
time (t), and the rate at any instant is given by the tangent to a
curve of the plot c=f(t).

44

Zero-order reactions are often seen for thermal chemical decompositions where the reaction
rate is independent of the concentration of the reactant (changing the concentration has no
effect on the speed of the reaction). The rate law for a zero-order reaction is
v=k

there

(6.9)

where v is the reaction rate, and k is the reaction rate coefficient with
units
of
concentration/time. If, and only if, this zero-order reaction (i)
occurs in a closed system,
(ii)
there is no net build-up of intermediates and
(iii)
are no other reactions
occurring, it can be shown by
solving a mass balance for the system that:
(6.10)

which

If this differential equation is integrated it gives an equation


is often called the integrated
zero-order rate law
(6.11)

where cA represents the concentration of the chemical of interest at a


particular time, and
cA0 represents the initial concentration. A reaction is zero order if concentration data are plotted
versus time and the result is a linear function. The slope is the zero order rate constant k. The
half-life of a reaction describes the time needed for half of the
reactant to be depleted. For
a zero-order reaction the half-life is given by
A first-order reaction depends on the concentration of only one reactant (a unimolecular
reaction). Other reactants can be present, but each will be zero-order.
A Products

(6.12)

The rate law for an elementary reaction that is first order with respect to

a reactant A is
(6.13)

k is the first order rate constant, which has units of 1/time. The
law is

integrated first-order rate

(6.14)

45

A plot of ln cA vs. time t gives a linear function with a slope of k. One


the concentration cA of reactant A at any time t

can easy express

(6.15)

where 0A c is the initial concentration of reactant A.


The half life of a first-order reaction (t ) is independent of the
given by

starting concentration and is

(6.16)

Kinetics of a first-order reaction characterizes also a radioactive decay,


describes the time taken for half the radionuclide's atoms to decay.

the Equation (6.16)

A second-order reaction depends on the concentrations of one second-order reactant, or


two first-order reactants. For a second order
reaction, its reaction rate is given by:
(6.17)

or

(6.18)

We will deal with the bimolecular reaction


A + B Products
supposing the same initial concentration of A and B reactants,
rate law for the second-order reaction is then

(6.19)
C0A=C0B=C0. The differential

(6.20)

Solving the differential equation, one can obtain


(6.21)

where c is the concentration of reactant at time t (CA=CB=C), and k is


the second-order
-1
-1
3
-1 -1
constant, which has dimension of concentration time (eg. dm mol s ). In this case, a
characteristic plot which will produce a linear function is 1/c vs. time t, with a slope of k (Fig.
6.1). The half-life equation for a second-order reaction dependent on one
secondorder reactant is
46

The half-life equation for a second-order reaction dependent on one


reactant is

second-order

(6.22)

Figure 5.1: Plot 1/c Vs. t.


4.0 MATERIALS & EQUIPMENTS:
4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8
4.9
4.10
4.11

250 mL Erlenmayer flask


50 mL Pipette
10 mL Pipette
5 mL Pipette
Burette
Water bath
Measuring Cylinder
Deionized water (DI water)
Ethyl Acetate
1.0 M HCl
0.5 M NaOH

5.0 PRODECDURES:
47

5.1

Obtain about 100 mL of deionized water, 30 mL ethyl acetate and 150 mL 1.0 M HCl in
a clean beaker (each separately). Allow these solutions to equilibrate in a 25 oC bath.
Into a dry 250 mL Erlenmayer flask pipette 50 mL of HCL and 50 mL of DI water. To initiate the
reaction add from a pipette 10 mL of ethyl acetate. Start the timer when the pipette is half
empty. Mix he solution thoroughly and keep it in the water bath.
As soon as possible, withdraw a 5 mL aliquot of reaction mixture and transfer it into a
erlenmayer flask which contains approximately 50 mL of water. The receiver should be prechilled in an ice bath to make sure that the hydrolysis is sufficiently slowed.
Titrate the diluted aliquot as soon as possible with the standard 0.5 M NaOH using
phenolphthalein as the indicator.
Repeat step 5.3 and 5.4 at 10 minutes intervals for one hour. Make sure that the pipette used
to withdraw each 5 mL aliquot is clean and dry.
At some convenience time titrate 2 or 3 aliquots of the equilibrated HCl so that the molarity at
25oC will be known exactly.
Repeat the above procedure using 100 mL 1.0 M HCl and 10 mL ethyl acetate as the reaction
mixture. This reaction will proceed more rapidly, so aliquots should be withdrawn at shorter
intervals (5 minutes). Duplicate runs should be performed if possible. An efficient student pair
be able to follow 2 or more proper space reactions at the same time.

5.2

5.3

5.4
5.5
5.6
5.7

6.0 RESULTS:
6.1

For each aliquot calculate C A (or a quantity proportional to C A). [The density of ethyl acetate is
0.901 g/mL at 250C and the molecular weight is 88.11].
Plot the ln CA Vs. t each set of data. Evaluate the acid-dependent rate constant, k H, in seconds
and explain your reading.

6.2

7.0 DISCUSSIONS:
7.1
7.2

Discuss and differentiate of zero order rate, first law order rate and second order rate.
Identify other example of second rate order.

8.0 CONCLUSION:
8.1

Based on the experimental procedure done and the results taken, write the conclusion
to this experiment.

EXPERIMENT 7
DETERMINE OF ELECTROCHEMISTRY FARADAYS LAW
1.0

OBEJCTIVES:
48

1.1 To calculate values for the Faraday constant and


Avogadros
experimental data.
1.2 To determine the number of moles of products formed in a redox
from experimental data.
2.0

number

of

reaction

INTRODUCTION:
Electrochemistry is the study of reactions that involve the movement of electrons:
these are oxidation-reduction reactions. In electrolysis, a reaction is driven in a
direction that it would not spontaneously go by applying a current (or voltage)
across the
cell. An electrochemical cell is the solution plus electrodes,
voltmeters, and rheostat that allow us to harness and measure the
current
produced by the reaction (a voltaic cell), or to apply
a current to make the
reaction occur (an electrolytic cell). In most electrolysis reactions, cations migrate to
the cathode
where they are reduced to elements by picking up electrons.
The
cathode is always negatively charged in an electrolytic cell
because electrons
are forced onto the cathode by the applied
voltage. The reaction(s) that occur at
the anode can be more complicated, and may involve anions, the anode itself, or
water, depending on which of these things is easiest to oxidize. A
diagram
showing a very simple electrolytic cell is shown in Figure 7.1.

Rheostat

Figure 7.1: A simple electrolytic cell. The electrons originate from the negative
terminal of the power supply and are forced onto the cathode (making it
negative). Cations migrate through solution to pick up electrons at the
cathode and thus get reduced to elements. Anions migrate the opposite way,carrying
the negative charge to the anode. Electrons are pulled off of
the anode
(making it positive)
into an ammeter (where we
can read the applied current) and
then back into the power
supply.
3.0

THEORY:
49

In 1832, Michael Faraday observed that the amount of substance undergoing


oxidation or reduction at an electrode in an electrochemical cell during electrolysis is
directly proportional to the amount of electricity that passes through the cell. This
statement is known as Faradays Law of Electrolysis. The quantitative unit of
electricity, now called the faraday, is the amount of electricity that reduces one gramequivalent weight of a substance at the cathode of an electrochemical cell and
oxidizes one gram-equivalent weight of a substance at the anode. This corresponds to
the gain or loss, and therefore the
passage, of Avogadros number of electrons.
The faraday is equivalent to 96,487 coulombs (ampere x seconds).
The equation for the reduction of copper (II) ions at the cathode

is:

Cu2+ + 2e- ---> Cu


One mole of copper ions needs two moles of electrons to form
atoms.

one mole of copper

1 mole of ions + 2 moles of electrons ---> 1 mole of atoms


63.55 g (copper ions) + 2 faradays ---> 63.55 g (copper atoms)
From this equation we see that 63.55 grams of copper plate
out onto the
cathode for every two faradays of electric charge. Of course, the same amount
of
copper would oxidize from the anode.
Faradays Law of Electrolysis suggests that 31.77 grams of copper plate out for
96,487 coulombs (one faraday) of electric charge.
4.0

5.0
5.1
5.2
5.3
5.4
5.5
5.6

MATERIALS & EQUIPMENTS:


4.1
Copper Sulphate solution (CuSO4 1.0M)
4.2
Distilled Water
4.3
50 mL Measuring cylinder
4.4
Copper Strips
4.5
5 Connector wires with crocodile clip
4.6
Ammeter
4.7
11 ohm rheostat
4.8
Power supply
4.9
Timer
4.10 Hair Drier
PROCEDURES:

Fill 150 mL 1.0 M CuSO4 solution in beaker.


Clean copper strips with sand paper and rinse with distilled water.
Dry the copper strips with hair drier.
Weigh he copper strips and record its mass.
Set a cell as shown in Figure 3.
Adjust the rheostat until 1 ampere and close the switch immediately and start the timer
to record the time.
50

5.7
5.8

After 30 minutes, on the switch and disconnect.


Copper strips removed and dry the strip before weighing it again.
6.0

RESULTS:

6.1

Write down your data as in Table 6.1.


Table 6.1: Data sheet of your experimental data.
Cathode
Initial Mass (g)
Final Mass (g)
Mass (g) (gain/loss)
6.2
7.0

7.1
7.2

By using the Faradays Law, calculate how many mol of electrons have been
transfer from cathode to anode.
DISCUSSIONS:

Briefly explain your understanding of Faradays Law.


By using the Faradays Law, calculate how many grams of cuprum (from the anode) have been
used. Compare with your experimental data.
8.0

CONCLUSIONS:
8.1

Based on the experimental procedure done and the results taken, write the
conclusion to this experiment.

51

Anode

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