Chem 201L Lab Manual

Department of Chemistry
CHEM 201L
Introduction to Chemical Analysis Lab.

Laboratory Manual
Spring 2014-2015
Table of Contents
Page
Safety Rules by the Environmental Health, Safety,
and Risk Management
Common Laboratory Equipment
A few tips to make life a little easier in Analytical

Chemistry Lab...
Check In Procedure
8
14
Locker equipment list
15
Experiment 1
Measuring the Density of Water
16
Experiment 2
Preparation of Primary Standard solutions and

Standardizing Acid and Base solutions
Analysis of a Mixture of carbonate and Bicarbonate
24
34
Experiment 5
Determining Iron Content in Foods by

Spectrophotometry
Study of an Organic Acid
Experiment 6
Distillation
52
Experiment 7
Recrystallization
59
Experiment 8
Chromatography
65
Experiment 9
Synthesis of Isoamyl Acetate
74
Experiment 10
????????????????????
79
Experiment 3
Experiment 4
Periodic Table of the Elements
28
41
Safety Rules by the Environmental Health, Safety,

and Risk Management
DO:
1. Wear lab coats (knee-length) and appropriate eye protection (minimum safety goggles).
2. Keep clean work places free of unwanted chemicals, biological specimens, radios, and idle
equipment.
3. Keep exits and passageways clear at all time.
4. Become familiar with the locations and operation of safety and emergency facilities such as the fire
extinguishers, first aid kit, emergency wash facilities, fire alarm pull stations, telephone, and
emergency exits.
5. Wash hands before leaving the laboratory.
6. Leave behind protective clothing (lab coats, gloves, etc.) when leaving the laboratory to eat.
7. Remove contaminated cloths immediately
8. Wash before eating, drinking, smoking, or applying make-up.
9. Pin or tie your hair (if long) up in a bun especially while working with chemicals, biohazards,
radioisotopes, or moving machinery.
10. Work only with materials when you know their flammability, reactivity, toxicity, safe handling,
storage and properly operating emergency procedures.
11. Perform all procedures involving the liberation of volatile materials or aerosols of a toxic or
flammable nature in a fume hood.
12. Place sharp objects (syringe needles, broken glass, blades, etc.) in a labeled rigid container before
disposal. Materials contaminated with bio-hazardous agents should first be autoclaved.
13. Keep wet hands and water away from electrical equipment.
14. Secure your compressed cylinders.
15. Perform a safety check at the end of each experiment - make sure that gas, water, electricity, vacuum
lines, air and heaters have been turned off and decontaminate any equipment or work areas which
may have been in contact with hazardous materials.
16. Lock laboratory when unoccupied.
17. Store coats, packs, etc., in areas provided, not around the lab bench.
18. Pay strict attention to all instructions before undertaking an experiment. If you do not understand,
ask.
19. Clean up apparatus and work areas at the end of the lab period.
20. Set up apparatus so that it is not necessary to reach through the assembly to turn water, gas or
electricity off.
21. Assemble apparatus so that control valves and switches will remain accessible if a fire should occur.
22. Be aware of what neighboring laboratory personnel are doing.
DO NOT
1. Wear open shoes (such as sandals, ballerinas, ballerinas with socks) in the lab.
2. Wear shorts, skirts and anything that shows the feet.
3. Block access to emergency equipment (eyewashes, safety showers and fire extinguishers).
4. Pipette by mouth.
2
5.
6.
7.
8.
9.
Pour water into acid

Return unused chemicals to stock bottles.
Run, walk in the lab.
Carry hazardous chemicals between the lab and storage rooms by hand. Use secondary containers.
Place chemicals where they will cause trip hazards, or are liable to cause personal injury. Reagent
bottles, empty or full should not be left on the floor.
10. Place chemicals near incompatible substances that may cause them to react.
11. Leave chemicals or experiments unattended.
12. Store food, food containers, drinking glasses in the laboratory.
13. Keep food in refrigerators at the laboratory.
14. Sniff or taste chemicals.
15. Smoke, eat, or drink, food, beverages or tobacco in laboratories.
16. Apply cosmetics or lip-balm in the laboratory.
17. Engage in horseplay or other act or mischief in the lab.
18. Perform unauthorized experiments.
19. Remove chemicals from the lab unless directed otherwise from the instructor/supervisor.
20. Use damaged or broken equipment when handling or experimenting with chemicals.
EHSRM: ext.2360
N.B: In case of violation of any of the above safety rules, you will be asked to leave the lab and you will
receive a zero grade on your report.
Environmental Health, Safety,

and Risk Management Procedures
Read carefully, it may save your life!
In Case of Fire
1. Remain calm Do not shout Fire.
2. Rescue: Rescue personnel who are in immediate danger. This step is usually performed
simultaneously with step 3 Alarm.
3. Alarm: Give the alarm Dial 5555 and inform operator of exact location of fire.
4. Contain: Close doors and windows to isolate fire and smoke from rest of the building.
5. Evacuate: Evacuate the building using the nearest exit (Do not use elevators). Do not reenter
the building until the alarm is silenced and you are told that it is safe to reenter
6. Extinguish: You may fight the fire if you have been trained to do so, your exit is assured and
that the alarm has been given.
7. Once the ERT / Beirut Fire Brigade arrives, they will be in charge until they declare the area
safe and leave the scene.
Hazardous Materials Emergencies: Chemical, biological and radioactive materials are
present in laboratories. If a hazardous material is spilled or released the following precautions
or actions are recommended:
If you are unsure about the danger of the material:
1. Do not approach the spill and avoid contact with the material. Avoid breathing gases, fumes
or smoke that may be generated. Vapours may be harmful even if there is no odour.
2. If others may be in danger, activate alarm or inform personnel to evacuate the area. Close
doors to contain the area of the spill.
3. From a safe location call the EHSRM x 2360 (during working hours) or the protection office
x 2400 (24 hours/day), describe the nature of the emergency.
4. Stay in a safe area near the vicinity so that you can assist emergency response personnel.
If you are certain that the spill or leak poses no immediate danger or personal injury
report it as in 3 above and:
1. Use absorbent material to keep the contamination from spreading or entering drains.
Absorbents such as sand, vermiculite, towel papers etc may be used.
2. Working from the outside in, absorb the spilled material; and using a shovel or dust pan place
the spilled material inside a plastic bag or container.
3. EHSRM personnel will advise on further actions.
If the spill is in a lab, shop or chemical storeroom:
1. Evacuate all personnel from the room.
2. Be sure hood/local exhaust is on.
3. If flammable liquids are spilled, disconnect the electricity to sources of ignition if possible.
4. Call EHSRM @ ext. 2360 to request additional assistance if you cannot manage the clean up
yourself.
4
If the spill is in a corridor or other public passageway:

1. Evacuate all people from the area. Close off area to keep others out.
2. Call the EHSRM at ext. 2360
3. Call Physical Plant @ ext. 2015 to request to have the air system in the area shut down (to
prevent contamination of other areas) and to request additional assistance.
Common Laboratory Equipment
Hardware
Glassware
A few tips to make life a little easier in

Analytical Chemistry Lab...
1. The lab reports (at least good ones) are going to take a while to write, so leave yourself
plenty of time before the due date to work up data and ask the TAs any questions you may
have. Also, dont forget to include little things like your name, your partners name, the
date...you get the idea.
2. Dont be messy! Make sure the balance area and your work space are clean before you
leave. Please wash any glassware you may borrow before you return it to the stock room
(this will keep the TAs happy and that's always a good thing!)
3. Dont use tap water for ANYTHING! (Except washing out the sink). Always use Dl water
in your experiments. The tap water is full of minerals and it will leave deposits on your
glassware. Its fine to rinse them with tap water before you put them away, but always
rinse with Dl water after tap. Also, dont dry your glassware with paper towels; they are
full of lint and will leave your glassware dirty.
4. Never pour anything down the drain unless specifically instructed to by the TA. If in
doubt, ask how something should be properly disposed of.
5. Pay attention in the pre-lab lecture. There is a reason that your TAs are up there talking, so
please listen, take notes if you wish, but DO NOT start setting up for the experiment. It
really irritates a TA when they have to answer a question because you didnt get the
answer from the lecture as you were too busy to pay attention, or worse yet, you hurt
someone because you didnt hear the safety precautions.
6. A few general lab hints:
a. Make sure the stopcock on your burette is closed before you start filling it. (It tends to
make a huge mess if it's open.)
b. Never pipette anything directly from the stock solution because you may contaminate
it; instead pour only the amount stated on the reagent bottle into a clean beaker and
pipette from there. If you get too much, share with those around you.
c. Put a sheet of white paper behind your burette to make the meniscus easier to read,
and put a white sheet of paper under your titration samples when using a color
indicator. Also when using a color indicator, if you think youve reached the endpoint,
but are not quite sure, add an extra drop of indicator and note the color when it first
hits the solution. If it turns the color of your endpoint immediately, youre finished.
7. Always bring a calculator to lab in case you need to do a quick calculation. One copy of
Harris is available for use in the laboratory. A word of warning: be careful with your
calculator in lab. Organic solvents will eat the plastic, and acids will ruin the LCD screen
(this goes for cell phones, MP3 players, PDA's, etc).
8. Always follow all the safety rules. The TAs dont like running around telling students to
put their safety glasses on their face, or to go home and put on pants or closed toed shoes.
Safety is JOB 1 for everyone in any laboratory, so build good habits.
9. This is probably one of the first upper level chemistry labs you have been in; youve paid
your dues with cookie-cutter gen. chem. labs so wed really like for you to explore the
chemistry were presenting. We want to teach you a whole new way of thinking that you
can apply not just to chemistry, but to your everyday life as well. We encourage lots of
questions, so utilize the TAs and if we dont know the answer, well find someone who
does. Dont be afraid to work together on common problems; discourse is a major part of
science. If you have questions, ask each other. This is a great way to learn tough material.
Have an enjoyable semester, and remember, even though the labs may be a lot of work,
we want you to have fun too.
Using the Analytical Balance

Electronic balances have no weights and the actual balancing is done by an electronic circuit.
The balance functions are controlled by a single bar which is located along the front of the
balance. This bar acts as an on/off switch and as a zero or adjusting switch. Above the control
bar is a digital display window which shows the weight currently being measured by the balance.
Precautions when weighing
Keep the balance clean.
Do not weigh chemicals directly on the pan. Use a small container or a vial.
Do not handle object being weighed directly with your bare hands, use gloves or a piece of
clean paper. Dirt or grease from the fingers will change the mass of the object.
Allow all objects or chemicals to attain room temperature before weighing, otherwise
convection currents will cause errors.
Perform all operations slowly and gently. The balance is a costly precision instrument and
must be treated with utmost care for it to continue functioning to its capability.
Operating procedure
1. Check that the pan is clean and all the sliding windows are closed.
2. Switching the balance on: Briefly press the control bar. All display elements light up for
several seconds; this permits a functional check of the display, then 0.0000 is displayed.
Ensure that the green pilot light in the left of the display goes off after the balance has
achieved stability. The result should always be read only after the pilot lamp has gone off.
3. Open the sliding window and place your container on the weighing pan, then close the
sliding window. Record the weight of your container to 0.0001 g.
4. Place the object to be weighed in the container and make sure you close the sliding
window. Record the weight to 0.0001 g. Liquids should not be poured within the balance
walls. Remove the container from the balance before pouring the liquid.
Using a Glass Buret

You will be using 25 or 50 mL burets. Graduations go from 0 at the top to 25 or 50 at the
bottom. You should be able to read these to an accuracy of 0.02 mL (i.e., 2 decimal places).
Before you use a buret, be sure that it is clean.
1. Fill the buret with the solution to be used and remove the funnel.
2. Remove any air bubbles from the tip of the buret. (Open the stopcock fully and tap the
buret at the bottom).
3. Wait 20 seconds before reading, to allow for drainage from the sides of the buret.
4. Read and write down the initial volume (Vinitial).
5. Add the required volume.
6. Read and write down the final volume (Vfinal).
7. The volume added (Vadded), will be (Vadded = Vfinal - Vinitial).
It is not necessary to set the level exactly at the zero. This can often be too time-consuming. But
it is absolutely necessary to record both the initial reading and the final reading to two decimal
places.
Readings
-Eye level parallel to meniscus (to avoid parallax)
-Read bottom of meniscus
-Interpolate to nearest tenth between two marks (0.01 mL for our 50 mL burets): uncertainty
in reading is 2 tenths of mark unit (0.02 mL for our 50 mL burets)
-Use white paper (with heavy black line) behind buret to read meniscus
-Drain buret slowly to avoid streaking and beading of solution
Endpoint
-Stir solution fast enough to mix well, slow enough to not splatter
-Use white paper under flask
-At first appearance of color, begin recording volume after each drop
-Near endpoint use half-drops:
Draw partial drop to tip of buret
Touch tip to side of flash just above solution
Swirl solution across point of contact to mix in partial drop
Record volume after each addition
Volumetric flasks
Volumetric flasks are designed to contain a specific volume of liquid when filled to the mark.
To prepare a solution using a volumetric flask, a known weight of solute or known volume of
another solution is added to the flask. (Note: Use a short-stem funnel to transfer solids to the
flask). Add distilled water until the flask is 2/3 full, and then agitate by swirling until the solid is
completely dissolved or the solution is thoroughly mixed. At this point more water should be
added to the flask until the liquid is 5 mm below the marking line. The last amount of water
should be added with a dropper until the bottom of the meniscus is right on the line etched in the
flask (place paper behind). Reading the meniscus position is crucial for all liquid measurements.
10
The correct way to do it is to keep your eye at the same level as the surface of the liquid (place a
white paper behind the scale to improve visibility). Once the proper amount of water has been
added, cover the flask with a stopper and complete the mixing by repeated inversions with
swirling and shakings in between. (Note: Keep your forefinger on the stopper at all times).
Pipets
A suction bulb will be used to fill the pipet. This bulb has three buttons, labeled A, S and E
which are abbreviations for aspirate, suction and empty respectively.
1. First squeeze the suction bulb (by pressing on the bulb and the A button at the same
time), then attach it to the tip of the pipet sealing it firmly to the rubber sleeve.
2. Then place the tip of the pipet below the surface of the liquid.
3. Press the S button and fill the pipet with the solution (making sure no air bubble is
withdrawn) until the liquid level is well above the mark on the upper part of the pipet but
making sure nothing enters the bulb itself. (WHY?)
4. Adjust the level of the liquid in the pipet till the bottom of the meniscus is tangent to the
upper graduation of the pipet while having your eyes at the same level as the graduation.
5. Remove the pipet with the bulb still attached to it and wipe the outside of the pipet with
a paper towel.
6. Place the pipet on top of the container in which you need to dispose your solution in, and
while touching the inner wall of the container, press the E button and empty the liquid.
Keep the pipet touching the inner wall of the container around 10 seconds after emptying
it to remove any drops adhering to the tip. A small amount of liquid will remain in the
tip. Do not blow this out. The pipet is calibrated to deliver the required volume with this
last drop remaining in the tip.
Graduated cylinders
Graduated cylinders are designed for measuring volumes of liquids. They are accurate to 1%.
You will be using cylinders of capacity 10, 25, 50 and 100 mL. To use a graduated cylinder:
1. Fill the cylinder to the required level.
2. Read the level at the bottom of the meniscus, always have your eye at the same level as
the surface of the liquid (place a white paper behind the scale to improve visibility).
3. Empty the cylinder, drain for 15 seconds.
Precision
The term precision describes the reproducibility of results. It can be defined as the agreement
between multiple measurements that have been made under the same conditions. The precision
of a set of measurements is related to the deviation of the data set from the arithmetic mean
(average).
Determination
Value of Individual
Number
Determination (Data Set)
1
0.315
2
0.321
3
0.320
Average (or mean value)
0.319
11
Deviations From
Mean Value
0.004 (=ABS(0.319-0.315))
0.002 (=ABS(0.319-0.321))
0.001 (=ABS(0.319-0.320))
0.007
= 0.002
3
So the average is 0.319 with an average deviation of 0.002.

Or, in terms of percent average deviation (precision or relative deviation)
=

0.002
100 =
100 = 0.6%
0.319
When reading any graduated scale, the precision of a single measurement is obtained by
dividing the value of the smallest division by two.
precision = smallest division / 2
Accuracy
The term accuracy expresses the closeness of an experimental value to a theoretical value, or
to its accepted value. The difference between accuracy and precision is very important in
experimental sciences. Accuracy involves a comparison with respect to a true or accepted value,
whereas precision considers the reproducibility (or smallness of the deviations). Normally,
higher precision in a series of measurements leads to higher accuracy in their average.
Sometimes you may have good precision in the measurements, but a poor accuracy an error in
calibration can cause measurements to be consistently too low or too high by some factor.
Significant figures
The number of significant figures is the minimum number of digits needed to write a given
value in scientific notation without loss of accuracy. The simplest way of indicating the
uncertainty in a measurement is by the method of significant figures. In any measurement, all the
figures which are certain plus one additional digit which is uncertain are used to express the
number; for example, a volume measured from a buret may be written as 13.05 mL. This number
contains four significant figures. The first three digits (13.0) are certain, while the fourth digit (5)
is uncertain. The uncertainty in the last digit is not defined.
The number 234.6 or 2.346102 has four significant figures. But the number 234.60 or
2.3460102 has an extra digit after the 6 and therefore has five significant figures. The number
2.346102 has four significant figures, it can be written as 0.02346, which also has four
significant figures. The leading zeros simply define the decimal point, they are NOT significant.
Zeros are significant when they occur:
1. in the middle of a number, e.g. 2.03 has three significant figures;
2. at the end of a number, on the right side of the decimal point, e.g. 2.030 has four significant
figures.
Numbers finishing with zero(s), like 12300, do not give a good indication as to how many
significant figures the number has. It could mean any of the following:
1.23104 three significant figures
1.230104 four significant figures
1.2300104 five significant figures
12
When calculating the result of addition and subtraction, use the lowest decimal place to
determine the significant figures of the sum:
47.4
4.32
0.0245
51.7445 = 51.7 = 5.1710
When calculating the result of multiplication, division, or other mathematical operations like
square root, Log, ln, sin, cos,... the result may contain as many significant figures as does the
involved quantity that has the least:
47.4 0.0025 5.268102 3.00 = 0.0021
number of significant figures
When addition or subtraction are involved in a calculation with multiplication, division, or other
operations, the rules must be applied to each individual step.
When taking a logarithm of a quantity, the number of digits to be written after the decimal
point equals the number of significant figures in the quantity. For example, the natural logarithm
of 10.0 must be reported to 3 decimal places because 10.0 has three significant figures.
Ln(10.0) = 2.303
Conversely, when a quantity is involved as the exponent in a calculation, the answer for that
operation must be reported with a number of significant figures equal to the number of decimal
places in the quantity. For example, when the pH of a solution is reported to be 4.32 (two
decimal places), the concentration of H3O+ ion in that solution is obtained by computing the
operation 10-4.32 and must therefore be written 0.000048 (two significant figures).
Concentration of H3O+ = 10-4.32 = 4.8 10-5 M
13
Check In Procedure
Open your assigned desk and remove all contents and place them on the benchtop. Check the
contents against the equipment list provided. Be sure that glassware is not cracked, chipped, or
otherwise damaged. Remove extra items from the locker and give them to the TAs. Obtain
replacements for shortages from the TAs.
NOTE: Check out will be held during the last week of classes. Details will be explained at that
time. You must check out if you drop the course before the end of the semester. See your TA for
instructions. A LBP 15,000 penalty will be assessed for failing to check out in addition to
anything lost or broken from the locker.
If you check out properly, a breakage allowance will be applied to any charges you have incurred
for broken or lost items.
IMPORTANT: The University will not issue transcripts until outstanding bills are settled.
I have read the above information and understand that I will be charged for excessive breakage
and/or an abandoned desk.
14
Chemistry 201L
Locker Equipment List
Check
IN
Check
OUT
2 Beakers , glass, 50 ml
2 Beakers, glass, 100 ml
1 Brush
1 Bottle, reagent
1 Bottle, washing
1 Buret column, 50 ml
1 Buret tip
1 Cylinder, graduated, 10 ml
1 Cylinder, graduated, 100 ml

4 Flasks, erlenmeyer, 100 or 125 ml
4 Flasks, erlenmeyer, 250 ml
1 Flask , erlenmeyer, 500 ml
1 Flask, volumetric, 10 ml
Check
IN
Name:__________________________
Family,
First
Check
OUT
6 Flasks, volumetric, 100 ml

1 Funnel, for buret
1 Funnel, glass, 75 mm diameter
1 Glass rod
1 Pair of tongues
1 Pipet filler
1 Pipet, graduated , 10 ml
1 Pipet, volumetric, 1 ml
1 Spatula or scopula
1 Stirring bar
6 Test tubes, 100 x 18
6 Test tubes, 180 x 15
1 Test tube holder
1 Test tube rack
2 Watch glasses
Student ID No:______________________
Student Imail:_____________ Locker No: ________
Lab Sec.:_________ Day: _______
I have received one desk key and the above items

Students Signature:____________________
Date:___________________
Instructors Signature:__________________
Date:___________________
15
Experiment 1
Objectives: The objective of this experiment includes:
1- Identifying the accurate balance in the lab.
2- Identifying the most accurate glassware.
3- Calculating the density of an unknown solution.
Introduction:
Volumetric glassware used in laboratories is probably one of the most important
"tools of the trade". They are containers that have been calibrated at a specific
temperature to deliver or contain very precise amounts of liquid.
Examples of
volumetric
glassware
include
burets,
pipets,
and
volumetric
flasks.
For the first part of this experiment, we will compare the measuring accuracy of
different volumetric glassware.
Beginning Question: What is the best way to measure the density of water?
Volumetric glassware can be used to determine the density of water. Density of a material
is defined as its mass per unit volume. Different materials usually have different
densities. The density of water is dependent on the dissolved salt content as well as the
temperature of the water. Thus, tap water, distilled water and sea water have different
densities as will be observed in the second part of todays experiment.
=
Another important thing that you will learn in this experiment and explain is errors. In science,
error is defined as the limitations that prevent any experiment from producing an exactly correct
value of the phenomena being observed. Error is different from a mistake, which is simply not
following the procedure you should. All experiments are affected by error, even those that are
carried out by really good scientists using state-of-the-art equipment. Error cannot be eliminated,
only minimized.
We group error into two types:
Random error is observed when repeated experiments give slightly different results.
Random error is a result of the limitations of instruments to produce exactly the same
result each time. Data that has a minimal amount of random error is said to be precise.
Systematic error is observed when an experiment produces results that are consistently
too high or too low. Systematic error is the result of instruments that are not properly
calibrated or an experimental design that is flawed. Data that has a minimal amount of
systematic error is said to be accurate.
To talk about random errors, one of the best ways to evaluate it is to use a statistical measure
called standard deviation. The standard deviation is a measure of the spread of value in a data
set. Thus, the greater the standard deviation, the greater the random error.
16
There are a variety of ways to calculate standard deviation.

(a) In Excel and most spreadsheet programs you can type all of the data values into a
column, then in the next row type =stdev( then select all of your data with the
mouse and hit Enter.
(b) Using a TI-83 or 84 calculator, hit the STAT key, select EDIT, then enter your data in
the L1 column. Then hit the STAT button, select CALC, 1-VarStats. The value that
comes up as Sx is the standard deviation. Note that this also gives you the mean
value, labeled as .
Procedure:
I.
Determining the Accurate Balance
Out of two analytical balances present in the lab, your instructor will assign you
which to use for this part of the experiment. One of these balances is inaccurate
and you have to determine which. Ask the instructor which balance to use.
1. Weigh a clean and dry 100 mL beaker on the assigned analytical balance and
record the exact mass in the report.
2. Using a 10 mL volumetric pipet, transfer 10 mL of distilled water to the 100
mL beaker and weigh the beaker with its contents.
3. Record the exact mass in the report form and calculate the mass of the 10 mL
water.
Note: Remember to read the volume of water so that the bottom of the water meniscus
(curved surface) is resting on the measuring line. Also remember to bring your eye to the
same level as the mark.
4. Empty your beaker, dry it with a paper towel, and repeat steps 1 to 3 two more
times for a total of 3 trials.
5. Calculate the density of water for each trial. Calculate the mean and the
standard deviation of these values.
6. Write all of your density values and the mean on the whiteboard.
7. Wait until everyone has posted their data on the board and copy them to your
report.
8. From the results, determine which balance is the accurate.
17
II.
Comparing the Measuring Accuracy of Different Volumetric Glassware.

Two balances will be used in this part. One is the accurate one you determined in part I,
and the other is assigned by the instructor. Both are accurate. You can use any.
1. Weigh a clean and dry 100 mL beaker on one of these analytical balances and record the
exact mass in the report.
2. Using a 100 mL graduated cylinder, transfer 10 mL of distilled water to the 100 mL
beaker and weigh the beaker with its contents.
3. Record the exact mass in the report form and calculate the mass of the 10 mL water.
Note: Remember to read the volume of water so that the bottom of the water meniscus
(curved surface) is resting on the measuring line. Also remember to bring your eye to the
same level as the mark.
4. Empty your beaker, dry it with a paper towel, and repeat steps 1 to 3 two more times for a
total of 3 trials.
5. Calculate the density of water for each trial. Calculate the mean and the standard
deviation of these values.
6. Repeat steps 1 to 5 using a 50 mL beaker instead of the 100 mL graduated cylinder.
7. If you used the inaccurate balance in part I, then repeat steps 1 to 5 using 10 mL
volumetric pipet instead of the 100 mL graduated cylinder. Otherwise, use the data you
obtained in part I.
8. From your results, determine which glassware is the more accurate.
III.
Determining the Density of an Unknown Solution
1. Obtain an unknown aqueous salt solution from your instructor and record its number in
the report form.
2. Repeat steps II. 1 to II. 4 using the most accurate glassware determined in part II.
3. Calculate the density of your unknown solution for each trial. Calculate the mean density
of your unknown.
Reference: J. Chem. Educ., 2012, 89 (10), pp 13051307
18
Student Name______________
Date_____________
Student ID #_______________
Section___________
Experiment 1

A. Purpose:
B. Data and Calculation:

I.
Determining the Accurate Balance
Balance 1: _ ____________
Student
1
2
3
4
5
6
7
8
9
10 mL volumetric pipet
Mean
Standard deviation
average
Balance 2: _ ____________
Student
1
2
3
4
5
6
7
8
9
10 mL volumetric pipet
Mean
Standard deviation
average
According to the class data, which analytical balance is the more accurate? Why.
19
II.
Comparing the Measuring Accuracy of Different Volumetric Glassware

1. Using a 100 mL graduated cylinder:
Mass of the
empty 100
mL beaker
Mass of 100
mL beaker +
H2 O
Mass of H2O
Volume
Density of water
(record to 4
decimal places)
Mean density = _________________________

Standard Deviation = ____________________
2. Using a 50 mL beaker
Mass of the
empty 100
mL beaker
Mass of 100
mL beaker +
H2 O
Mass of H2O
Volume
Density of water
(record to 4
decimal places)
Mean density = _________________________

3. Using a 10 mL volumetric pipet:
Mass of the
empty 100
mL beaker
Mass of 100
mL beaker +
H2 O
Mass of H2O
20
Volume
Density of water
(record to 4
decimal places)
Mean density = _________________________

Questions:
1. Which piece of glassware is best at measuring the density of water?
2. What two aspects of the data set you cited in Question 2 define it as best?
3. What does standard deviation measure?
4. (a) Did your measurements exhibit random error? Briefly explain. (Hint: Remember that
any deviation between values indicates random error)
(b) What is the source of random error in your measurements?
(c) Did your measurements exhibit systematic error? Briefly explain.
(d) What is the source of systematic error (if observed) in your measurements?
21
(e) Did any of your measurements represent mistakes rather than error?
5. Looking at the data obtained for the 50 mL beaker, is it really necessary to report all four
digits in the answer? Why or why not?
III.
Determining the Density of an Unknown Solution
Unknown number: ______________

Balance used: __________________
Glassware used for delivering the unknown solution: ________
Data and calculation:

Mass of the
empty 100
mL beaker
Mass of 100
mL beaker +
H2 O
Mass of H2O
Volume
Density of
unknown
(record to 4
decimal
places)
Mean density for the unknown = _________________________
22
1. Does your data for the salt water exhibit random error? Is the error large or small
compared to the average value?
2. In this portion of the experiment you do not know the accepted value of the density of
this sample beforehand. What could you do to ensure that your experimental procedure
gave accurate results?
3. Is the density of water the same for this salt water as it was for pure (deionized) water?
Why was it important that everyone used pure water in the initial experiment?
4. (a) What does the standard deviation of the salt water data tell you about this data?
(c) Does the standard deviation tell you anything about potential systematic error in the
salt water data?
23
Experiment 2
Preparation of Primary Standard Solutions and
Standardizing Acid and Base Solutions
Objectives: The objectives of this experiment are:
1- To prepare a primary standard solution, sodium carbonate (Na2CO3).
2- To standardize a hydrochloric acid solution using the prepared primary
standard Na2CO3.
3- To calculate the concentration of an unknown Na2CO3 solution.
Introduction
A primary standard is a standard that is accurate enough that it is not calibrated. For a
compound to be considered as a primary standard it should have several important
characteristics, the most important of which are high purity, stability, low hygroscopicity, high
solubility, and high molar mass. A primary standard solution is a solution of known
concentration made from a primary standard. Primary standard solutions are used in determining
the concentrations of other solutions to an extremely high accuracy. They are typically used in
titrations and other analysis techniques as standardization solutions.
A secondary standard solution, such as HCl solution, is a solution which must be
standardized first against a primary standard, but afterwards, it will be stable enough for
titrimetric work (Titration).
Titration involves the gradual addition of a solution of accurately known concentration
(standard solution) to another solution of unknown concentration (or vice versa), until the
chemical reaction is complete. Titrations are based on reactions which go to completion rapidly.
A reaction is complete when stoichiometric amounts of the reacting substances are combined.
This is the stoichiometric point (equivalence point) in the titration. The equivalence point is
detected visually using an indicator. An indicator is a substance (added at the beginning of the
titration to the flask) that changes color at (or very near) the equivalence point. The point where
the indicator actually changes color is called the end point of the titration.
In this experiment, the primary standard to be used is sodium carbonate, Na2CO3 (molar mass
= 105.99 g/mol), a base, by which a hydrochloric acid solution will be standardized. The
chemical equation of the reaction is:
2HCl(aq) + Na2CO3(aq) CO2 (g) + 2NaCl(aq) + H2O(aq)
The reaction above generates CO2, which dissolves into the solution to generate an acid. The
presence of dissolved CO2 thus interferes with the pH and the detection of the end point of the
titration. However, the CO2 can be driven off by boiling the solution, enabling an accurate
titration.
24
In this experiment, the indicator to be used is bromocresol green, which is blue in acidic
solutions. Bromocresol green changes from blue, through green, to yellow. The proper stopping
point is at the intermediate green color, which corresponds to a pH f 4.7.
Procedure
I.
Preparation of the primary standard Na2CO3
1. Obtain a bottle containing ~ 1 g of dry Na2CO3 and weigh it with the cap on the
analytical balance. Record the mass in Table 2.I.
2. Transfer the solid Na2CO3 to a 100 mL volumetric flask using a funnel, re-stopper
the bottle and weigh it. Record the mass in Table 2.I.
3. Rinse the funnel to wash any sticking solid using a washing bottle and add more
distilled water into the volumetric flask to dissolve the Na2CO3 (1/2 its capacity).
Swirl the flask; make sure to dissolve the solid completely. Add more water (2/3)
and swirl again. Dilute to the mark carefully, stopper or cover with a parafilm paper
and invert several times with swirling to homogenize the solution.
II.
Standardization of HCl with Na2CO3

1. Obtain in a beaker around 100 mL of the primary standard Na2CO3 solution and
record its exact concentration in the report form.
2. Obtain in another beaker around 200 mL of HCl solution and cover with a watch
glass.
3. Rinse your buret, after washing it with distilled water, with few mL of the HCl
solution; allow some solution to flow out through the lower end. Fill the rinsed
buret with HCl, make sure that the tip is filled with no air bubbles.
4. Pipet a 10 mL aliquot of the primary standard Na2CO3 solution into a 125 mL
Erlenmeyer flask. Add 25 mL of distilled water and two drops of bromocresol green
indicator. Record the buret reading (use a white card as background to facilitate
reading the buret). Put a white tile below the Erlenmeyer flask and start titrating by
adding HCl continuously and with constant swirling of the flask until a change of
color from blue to faint green. Report the volume of acid at this point and keep the
solution as reference for color for the other titrations.
5. Repeat the titration slowly three more times. Record data in Table 2.II.
III.
Determining the Concentration of an Unknown Na2CO3 Solution

1. Pipet a 25 mL aliquot of the unknown solution into a 125 mL Erlenmeyer flask.
Add two drops of the needed indicator (either phenolphthalein or bromocresol
green). Record the buret reading (use a white card as background to facilitate
reading the buret). Put a white tile below the Erlenmeyer flask and start titrating by
adding HCl or NaOH continuously and with constant swirling of the flask until a
change of color according to the indicator being used is observed. Record the lower
reading of the buret.
2. Repeat the titration slowly three more times. Record data in Table 2.III.
Reference: Harris, Quantitative Chemical Analysis, 7th Ed.
25
Date_____________
Student ID #_______________
Section___________
Experiment 2
Preparation of Primary Standard Solutions and

Standardizing Acid and Base Solutions
Purpose:
I.
Preparation of the primary standard Na2CO3
Table 2.I: Data and calculation of the concentration of Na2CO3

Mass of vial + cap + Na2CO3
Mass of vial(empty) + cap
Mass of Na2CO3
Volume of solution
M Na2CO3 = ___________________
II.
Standardization of the HCl Solution

Table 2.II: Data and calculation of the concentration of HCl solution
Trial
Upper buret
Lower buret
Volume of HCl
reading (mL)
reading (mL)
(mL)
1
2
3
Volume of Na2CO3 aliquot =_________________
26
Volume of HCl
for blank (mL)
V HCl = ___________________________________
III.
HCl (average)=
____________________________
Determining the Concentration of an Unknown Na2CO3 Solution

Unknown # =
Volume of unknown (aliquot) =
Table 2.III: Data and calculation of the concentration of unknown Na2CO3 Solution
Trial
Upper buret reading
Lower buret reading
Volume of HCl
(mL)
(mL)
1
2
3
V HCl (average) = _______________________

M unknown (average) = _____________________________
27
Experiment 3
Analysis of a Mixture of Carbonate and Bicarbonate
Objectives: The objectives of this experiment are:
1- To determine the total alkalinity of a solid mixture.
2- To determine the percentages of carbonate and bicarbonate in an unknown.
Introduction
A carbonate is a salt of carbonic acid, characterized by the presence of the carbonate ion,
CO32-. A bicarbonate ion (hydrogen carbonate ion) is an anion with the empirical formula
HCO3-. The bicarbonate ion carries a negative one formal charge and is the conjugate base of
carbonic acid H2CO3 and the conjugate acid of CO3 2 , the carbonate ion. End points to
distinguish individual constituents with mixtures such as NaHCO3 (Molar mass = 84.077) and
Na2CO3 (Molar mass = 105.99) are difficult to recognize using indicators or dyes. However, by
using the technique of back-titration with analysis of a mixture (through a little help from
precipitation chemistry), it can be feasible.
The procedure today involves two titrations for an unknown mixture of sodium carbonate and
sodium bicarbonate.
First, total alkalinity (defined as total base concentration, in this case [HCO3- + 2[CO32-])) is
measured by titrating the mixture with standard HCl to a bromocresol green end point:
HCO3-(aq) + H+(aq)
H2CO3 (aq)
CO32- (aq) + 2H+(aq)
H2CO3 (aq)
In this first titration, there is no way to differentiate between the second and first reactions, so
the endpoint of the reaction is for both of the reactions, together.
Second, the original carbonate concentration of the unknown is determined by exploiting a
number of methods, including selective precipitation. A fresh aliquot of unknown will be treated
with an excess of standard sodium hydroxide, converting all HCO3- to CO32- :
HCO3- (aq) + OH- (aq)
CO32- (aq) + H2O
Your sample then consists entirely of CO32-, which will be precipitated by adding excess
barium chloride:
The excess NaOH is then immediately titrated with standard hydrochloric acid to determine
how much bicarbonate had been originally present in the sample. From this value and the total
alkalinity, the original carbonate concentration can be easily calculated.
Reference: Harris, Quantitative Chemical Analysis, 7th Ed.
28
Procedure
I.
Preparation of the Unknown

1. Obtain a vial containing an unknown mixture of carbonate/bicarbonate from your
instructor and record its number in Table 3.1.
2. Weigh the vial with the content and the cap accurately ( 0.1 mg) and record the mass
in Table 3.1.
3. Transfer the unknown to a clean 250 mL volumetric flask by means of a funnel. Rinse
any solid stuck on the funnel with distilled water into the volumetric flask but do not
rinse your vial. Remove the funnel.
4. Weigh ( 0.1 mg) the empty vial with the cap and calculate the mass of your
unknown. Fill your volumetric flask with around of its volume with distilled water
and swirl to dissolve the solid.
5. Fill half of the flask with distilled and swirl. When all dissolves, add distilled water to
the mark, stopper the flask and homogenize the solution.
II.
Total Alkalinity Determination:

1. Pipet a 10.00-mL aliquot of unknown solution into a 250 mL Erlenmeyer flask.
2. Titrate with standard 0.10 M HCl, using bromocresol green indicator as in
Experiment 2 for standardizing HCl, from blue to green.
3. Repeat this procedure with three more 10.00 mL aliquots. Record data in Table 3.2.
III.
Bicarbonate Content Determination

1. Pipet 10.00 mL of the unknown and 20.00 mL of standard 0.10 M NaOH into a 250
mL Erlenmeyer flask.
2. Swirl and add 4 mL of 10 wt% BaCl2, using a graduated cylinder. A white precipitate
is observed upon the addition of BaCl2.
3. Swirl again to precipitate BaCO3.
4. Add 2 drops of phenolphthalein indicator (a pink solution with white precipitate is
observed), and immediately titrate with standard 0.10 M HCl.
5. Repeat this procedure with three more 10.00 mL samples of unknown. Record data in
Table 3.3.
Calculations
1. From the results of step 2, calculate the total alkalinity (concentration and moles).
2. From the results of step 3, calculate the bicarbonate concentration and number of moles.
3. Calculate the concentration of carbonate in the sample.
4. Calculate the mass of carbonate and bicarbonate in the whole sample as well as their
percentages in the sample. . Express the composition of the solid unknown in a form such
as 63.4 wt% Na2CO3 and 36.6 wt% NaHCO3.
29
Date_____________
Student ID #_______________
Section___________
Experiment 3
Analysis of a Mixture of Carbonate and Bicarbonate

Purpose:

Table 3.1 Preparation of the unknown (# ________)
Mass of vial + cap + unknown
Mass of vial (empty)+ cap
Mass of unknown
Volume of solution
Table 3.2 Total alkalinity determination

Trial
Upper buret reading

(mL)
Lower buret reading

(mL)
1
2
3
Please show a detailed calculation:

Volume of unknown aliquot =___________
M HCl=______________________________
30
Volume of HCl
(mL)
V HCl = ___________________________
n unknown (total alkalinity) =__________________
M unknown (total alkalinity)= ___________
Table 3.3 Bicarbonate titration

Trial
Upper buret reading

(
mL)
Lower buret reading

( mL)
Volume of HCl
( mL)
1
2
3
Volume of unknown aliquot =___________

M HCl=______________________________
V HCl = ___________________________
Calculations (Show a detailed calculation):

Molarity of NaOH =_________________________________
Volume of NaOH aliquot=____________________________
31
# of moles of NaOH = ______________________________
# of moles of NaOH unreacted =____________________________
# of moles of NaOH reacting with bicarbonate =________________
# of moles of bicarbonate = _________________________________
Molarity of bicarbonate = __________________________________
Mass of bicarbonate = _____________________________________
% mass of bicarbonate in unknown= ___________________________
# of moles of sodium carbonate = _____________________________
Molarity of sodium carbonate = _______________________________
Mass of carbonate = ________________________________________
32
Questions:
1. If you added an insufficient amount of barium chloride, what would be the effect on your
measured values for the total alkalinity and the bicarbonate and carbonate
concentrations?
2. If barium carbonate were not insoluble, what would be the effect on your measured
values for the total alkalinity, and the bicarbonate and carbonate concentrations?
3. Would you be able, from your measurement, to tell if we had given you a mixed sample
of, for example, sodium carbonate and potassium bicarbonate?
33
Experiment 4
Determining Iron Content in Foods by Spectrophotometry
Objective: The principle objectives of this experiment are to:
1- Prepare a calibration curve for iron thiocyanate using a spectrophotometer.
2- Calculate the concentration of iron in an unknown solution and in foods.
Introduction
Iron is an important mineral in our diets. Although considered a trace mineral (one that is
needed in relatively small quantities), diets lacking iron can contribute to the deficiency
condition known as anemia. Certain foods, such as raisins, liver, and spinach, are natural sources
of iron. Other foods, such as breads and cereals, are fortified with additional iron.
The test for the iron (III) ion is done in solution and is based on the following reaction:
Fe3+(aq) + SCN-(aq) Fe(SCN)2+(aq)
The deep read color of the iron (III) thiocyanate ion is directly related to the concentration of
iron (III) originally present in the solution. Iron in foods is in the form of either iron (II) or iron
(III). In this test, all iron in the original sample is either converted to iron (III) ions or is not
determined through the thiocyanate test.
The reaction of the iron (III) ion with the thiocyanate ion yields a reddish-brown complex ion
by the following equation:
Fe3+ (aq) + 6 SCN- (aq)
[Fe(SCN)6]3- (aq)
Reddish-brown
The presence of the colored ion allows for analysis by spectrophotometry.

Spectrophotometry is a method used to determine the amount of a particular substance present in
a sample by measuring the amount of color present. This method requires the use of a
spectrophotometer that electronically measures the intensity of light that is able to travel through
a sample (also known as transmittance). The instrument can then convert the amount of light
that was transmitted to the amount of light that was absorbed by the sample. The amount of
radiant energy a coloured solution absorbs (i.e., its absorbance) varies with the wavelength of
light, , passing through the solution. A plot of absorbance vs. wavelength is called the
Absorption Spectrum of the compound in the solution. The absorption spectrum of a coloured
compound will have at least one absorption maximum in the visible region. At this wavelength,
max, the substance absorbs more light energy than at other wavelengths. This means that at max
the spectrophotometer is most sensitive or responsive to that material. Thus to determine the
amount of a coloured substance present in a sample, the spectrophotometer is usually set at the
max for that substance; at this wavelength the smallest amounts can be determined.
The amount of light that gets absorbed by the sample is directly related to the concentration of
the colored analyte by Beers Law:
A = bc
where A = absorbance of the sample
= molar absorbtivity constant (unique for a particular chemical)
34
b = path length (or distance) through the sample

c = concentration
The absorbance value alone cannot be used to determine the amount of analyte present
without knowing the molar absorptivity for the analyte. If the sample size is kept constant, there
will be a linear relationship between the absorbance and the concentration that we can use to our
advantage. Therefore, a standard curve is prepared from a series of solutions that have been
prepared to contain a known amount of analyte. The standard curve is made by measuring the
absorbance of each prepared standard and plotting the absorbance vs. concentration of analyte
for each standard. The line generated can then be used to determine the amount of iron in the
food sample by comparing its absorbance value to the line.
Spectrophotometer:
Light
Source
Figure 4.2 General schematic of a spectrometer

White light emitted by the lamp (e.g. incandescent tungsten filament) is focused by the field
lens onto the objective lens. This lens focuses the white light on the diffraction grating, which
reflects light of a desired wavelength through the exit slit.
The diffraction grating is a plastic replica of a lithographically produced grating with typically
600 evenly spaced grooves per millimeter. The light impinging on the grating is dispersed into a
continuum of different wavelengths ranging from 330 nm (ultra-violet to violet) to 800-1050 nm
(infrared, limited by detector sensitivity). The chosen wavelength range is reflected onto a
screen with a slit cut into it. Any light not absorbed by the sample solution impinges on the
detector, where the intensity of the transmitted light is converted to an electric signal displayed
by the spectrophotometer. The detector currently used in most spectrometers is a silicon
photodiode. By varying the wavelength continuously or in increments while recording
absorbance (or transmittance), the absorption spectrum of the sample can be produced.
For several spectrometers, the 100% T or Zero A control regulates the amount of light passing
through the exit slit to the detector. The need for this light control arises from the fact that the
light source does not emit light of equal intensities at different wavelengths, and the photodiode
detector is not equally responsive to light of varying intensities. Also, the "blank" solution,
which is a solution containing all components of the sample except for the compound under
investigation, may itself absorb light of certain wavelengths. In order to measure the absorbance
35
due to a particular species in solution, such side effects that affect the % T reading must be
compensated for. Therefore, after the colourimeter has been turned on and allowed to warm up
for ~5 minutes, the "blank" solution is placed in the light path, and the reading is adjusted to
achieve this desired compensation. If a sample solution is now placed in the light path, any
change in the absorbance reading is due to the particular light absorbing species in the sample,
and the absorbance reading is a measure of that species present.
Procedure
I.
The Visible Spectrum
Paper
Figure 3: Experimental Set-Up for Part A

Place a white piece of paper into the sample holder. Observe and record the colour of the beam
every 50 nm from 650 nm down to 350 nm. Record the observations in Table 4.1.
You must get close to the spectrophotometer and prevent outside light from entering the sample
while trying to determine the colours.
II.
Preparation of a Food Sample
Pick one food from the following list: Broccoli, peas, cauliflower, spinach or beans (If you
want to try another type of food, please discuss it with your TA) and bring it to the lab in two
forms, the first as a fresh sample and the second cooked (Baked, steamed etc) but both finely
chopped or grinded.
1. Weigh out 2.5 g of your sample and record the weight in the report to four decimal
places.
2. Place the sample in a clean dry crucible.
3. Heat the sample over a Bunsen Burner until it has been reduced to an ash.
4. Allow sample to cool (in the meantime, start with part II)
5. After the sample has cooled, transfer the contents to a 50 mL beaker.
36
6. Pipet 10 mL of 2.0 M HNO3 to dissolve the iron(III) present in the ash and stir
gently for 5 minutes
7. Filter the sample quantitatively and by suction using no more than 5 mL of 2.0 M
HNO3 to aid in transfer.
8. Pipet 4 mL of the filtered solution to another container and keep it for use as the
blank.
9. Pipet 4 mL of the filtered solution to a clean 50 mL volumetric flask using no more
than 5 mL of 2.0M HNO3 to aid in transfer
10. Pipet 20 mL of 1.5 M KSCN to flask
11. Dilute to the mark with 2.0 M HNO3 and homogenize.
III.
1.
2.
3.
4.
5.
6.
Preparation of [Fe(SCN)6]3- Standard Solutions and Determination of Their

Absorbance
Clean five 50 mL volumetric flasks and label them 1 to 5.
To these flasks, pipet 0.50, 1.00, 1.50, 2.00 and 2.50 mL of 0.0010M Fe(NO3)3 (in 1
M HNO3) stock solution respectively.
To each flask, pipet 20 mL of 1.5 M KSCN.
Dilute to the mark with 2.0M HNO3 and homogenize the solution.
Prepare a blank containing everything except the KSCN.
Measure (using a spectrophotometer) the absorbance of the prepared standards at
max = 447 nm and record their values in Table 4.2.
Note: Zero the absorbance of the blank before reading the absorbance of each
solution.
IV.
Absorbance Measurements of the Prepared Food Sample

1. Measure the absorbance of the prepared food sample at max (447nm) and record
the value in Table 4.3.
2. If the absorption is higher than 1, dilute your sample accordingly and remeasure the absorbance at max.
V.
Absorbance Measurements of an Unknown Solution.

1. Clean a 50 mL volumetric flask
2. Add 20 mL of 1.5M KSCN to the flask using a pipette
3. Obtain an unknown from your instructor and record its number in Table 4.4.
4. Pipet 5 mL of your unknown Fe(NO3)3 (In 1 M HNO3) solution
5. Dilute to the mark with 2.0M HNO3 and homogenize the solution.
3. Measure its absorbance at max and record the value in Table 4.4.
References:
J. Chem. Educ., 2010, 87 (10), pp 10981101
J. Chem. Educ., 1995, 72 (7), p 649
37
Date_____________
Student ID #_______________
Section___________
Experiment 4
Determining Iron Content in Foods by Spectrophotometry

Purpose:

Table 4.1: Visible spectrum
Table 1: Colour observed for various wavelengths of white paper
Wavelength (nm) Colour Observed
650
600
550
500
450
400
350
38
Table 4.2 Calibration Curve of [Fe(SCN)6]3

max= ________________
Standard
Volume of Fe stock
solution
[Fe(SCN)6]3-
Absorption at max
Plot Absorbance versus concentration and attach the graph to the report. Show the equation of
the line and the regression.
Table 4.3 Iron content in food
Vegetable (fresh) =
Weight
Absorption at max
Absorption at max for diluted
sample if needed:
Dilution factor =
Concentration of iron
Table 4.4 Iron content in the unknown

Unknown #= ________________
Absorption at max
Absorption at max for diluted sample if
needed: Dilution factor =
Concentration
39
Vegetable (cooked)=
Use the standard curve to determine the iron (III) concentration of the food samples you tested
and your unknown.
Calculations/Questions:
1. Convert the concentration from mole/L to mg/L of Fe3+ in your food and unknown sample.
2. Determine the number of milligrams of Fe3+ in your food sample.
3. Determine an accepted value for the iron in the analyzed food.
4. Calculate the percent difference between your fresh and cooked sample.
5. For someone of your age sex, age and weight, what is the bodys daily requirement for Iron?
6. Discuss your bodys needs for iron. According to your results, what mass of the vegetable
analyzed would you have to consume to get your daily supply needs?
40
Experiment 5
Objectives: The principal objective of this laboratory exercise is to identify
an unknown organic acid through measurement of three of its
physical/chemical properties:
1- Acid dissociation constant (obtained via potentiometric
titration)
2- Equivalent weight (obtained via potentiometric titration)
3- Melting point range
Through these measurements you will learn to use a pH-meter and a melting point
apparatus. Analysis of your titration curves will employ the first and second derivative technique
to determine the end point of your titration. You will confirm the identity of your acid by mixed
melting point.
Introduction
An organic acid is an organic compound with acidic properties. The most common organic
acids are carboxylic acids, whose acidity is associated with their carboxyl group COOH. In
general, organic acids are weak acids and do not dissociate completely in water. Upon
dissociation in solvents other than water, they produce their conjugate bases. The produced
conjugate bases determine the acidity of the acids.
The strength of the acid is defined by acid dissociation constant, Ka. Due to the many orders
of magnitude spanned by Ka values, a logarithmic measure of the acid dissociation constant, pKa,
is more commonly used in practice. The larger the value of pKa, the smaller the extent of
dissociation. pKa can be found experimentally from the data accumulated during a
potentiometric titration using a pH meter. Potentiometric titration of organic acids is used to
determine the molecular weight of a carboxylic acid as will be studied in this experiment.
The pH meter, which is based on an electrochemical cell, gives a direct measurement of the
pH of a solution. The pH meter is essentially a potentiometer with electronic amplification to
permit measurement despite the very high resistance (10 7 - 10 8 ohms) across the glass electrode.
Our meters are Cyberscan pH-10 meters which require no warm-up time, and may be used
immediately on being turned on. Review Harris, section 15.5.
When potentiometric titration is combined with melting point determination, identifying the
unknown out of a given list of possibilities can be feasible. The melting point of a substance is
the temperature at which the material changes from a solid to a liquid state. A pure substance
melts at a precisely defined temperature, characteristic of every crystalline substance and
dependent only on pressure (though the pressure dependency is generally considered
insignificant).
To confirm the identity of an unknown, a mixed melting point is performed. During a mixed
melting point, a small amount of the sample is mixed with an equal amount of the suspected
compound and the mixed melting point is determined. If the melting point of the mixture does
not drop, then the reference substance that was added is identical to the sample (i.e. the sample
41
has been identified). If the melting point of the mixture is depressed, then the two substances are
not identical.
On page 50, you can find a list of organic acids. The unknown that you will receive is one of
the organic acids present in the list. The list gives the literature values of the pKa, the molecular
weight, melting point, and structural diagram of each acid.
There are three main parts in this experiment, which are discussed in detail in the
procedure section:
1. Potentiometric titrations (using a pH-meter) of your unknown acid (two repetitions)
2. Melting point determination of unknown
3. Mixed melting point to confirm the identity of your unknown
The colorimetric titrations are performed using your standard glassware. The potentiometric
titration requires a few hours of work and a well-functioning pH-meter (check with the TA if you
have problems with the pH-meter). The melting point range determination and mixed melting
point are relatively quick experiments and there are several melting point apparatus available in
the laboratory.
Note: You are ready to take a mixed melting point only when you have determined all of
the three properties of your unknown acid (pKa, equivalent weight, m.p.) and it is usually
done during the second lab period. The other experiments can be done in any sequence.
Reference: Harris, Quantitative Chemical Analysis, 7th Ed. Chapt.-Sect.: 9-3, 11-2, 11-5, 18-2,
18-3.
Procedure (Work in pairs)
Note: Stoichiometric point, equivalence point, and end point all mean the same thing in titrametric jargon.
a. Titration of the Unknown Acid:

It is important to realize that since we are using aqueous ethanol instead of water, the
ionization constants obtained are not the true aqueous constants. The values in 50%
ethanol are in nearly all cases 1 to 1.5 pKa units higher than in water.
1. Fast Titration:
a. Obtain the unknown acid from your TA and record its number in the report.
b. Weigh out a 0.3-0.4 g sample into a 400 mL beaker; record the masses to 0.1
mg. Remember to record the weighing in Tables 5.2 and 5.3, not just the
difference.
c. Dissolve the sample by stirring with 50 mL of 95% ethanol.
d. After the sample is completely dissolved, add 10 mL of distilled water (these
solvent volumes do not need to be exact). With this solvent mixture and the
addition of your 0.1 M aqueous KOH titrant, the solvent composition near your
titration endpoint should be 50% ethanol.
e. Place the pH-meter into the acid solution and measure and record its pH before
adding any KOH from the buret. You will need this value of pH later for your pKa
42
f.
g.
h.
i.
j.
calculations and to find the molecular weight of the unknown. Now you are ready
to perform the first (rough) of your potentiometric titrations.
Titrate this sample by adding ~0.5-mL aliquots of standardized KOH. Record the
new pH value after each addition of KOH. Most of the organic acids we are using
have a pH at the stoichiometric point in the range of 7.5-9.5.
Proceed with your titration until the pH becomes stable, usually in the range 10.512.0. In any case, go at least 10 mL beyond the stoichiometric point.
From this first titration, estimate the volume of KOH necessary to reach the
stoichiometric point (Vo; example: 30 mL) and calculate a Vo 2.0-mL range
(example: 28-32 mL). Also, calculate half the value of volume you needed to
reach the stoichiometric point (Vo/2; ex: 15 mL) and a range of Vo/2 1.5 mL (ex:
13.5-16.5 mL). Plot the titration curve while titrating. You may use your
laptops.
Attach the table of pH obtained versus volume added and plot a graph of the pH
versus volume. Show on the graph the pH at equivalence and the pH at half
equivalence.
When you are finished with the pH titration, rinse the electrode with distilled
water.
2. Slow Titration:
You will now perform a more careful duplicate titration.
Note: It is important that the mass of the second sample be very close to that of the first (max.
difference of 10 mg) so that the Vo/2 and Vo ranges will be close to those determined from your
first titration.
Perform the second titration (slow) as carefully as the first (fast), but be ready to adjust
the KOH addition to different speeds during the course of this titration.
a. Prepare the sample for titration as steps a to d in part 1.
b. As before, measure and record the initial pH before adding any KOH.
c. Start adding aliquots of 2-3 mL of KOH per addition step as long as you are still
far from the half stoichiometric point range you previously calculated (Vo/2; ex:
13.5-16.5mL). Record the new pH value after every addition of KOH. When
you approach this range, adjust the KOH addition to 0.1 mL and carefully record
the pH after every addition.
d. Once you have passed this range, start again adding aliquots of 2-3 mL of KOH
per addition until you approach the stoichiometric point range (Vo; ex: 28-32
mL). In this range adjust the KOH addition to about one drop and record the pH
after every addition. The purpose is to get accurate volume and pH data for
determining the endpoint using the first and second derivative method. The slow
addition of base should be suitable for the pH reading to stabilize before the next
drop falls; this is not easy.
e. At the end of this range, again accurately read the buret volume.
f. After this range start adding once more 2-3 mL aliquots of KOH per addition and
continue your titration until the pH stabilizes around 11-12. Record the pH after
every addition.
43
g. Attach the table of pH obtained versus drops added and plot a graph of the pH
versus volume. Show on the graph the pH at equivalence and the pH at half
equivalence.
h. When you are finished with the pH titration, rinse the electrode with distilled
water and re-immerse it in buffer.
i. Determine the exact end point by the method of second derivatives (described
below). For both the first and second titration, plot the pH versus volume of
KOH added. For the second titration only, plot pH/V versus V of KOH and
2pH/V2 versus V of KOH using the values of pH and V obtained in the
stoichiometric point range (Vo; ex: 28.5-31.5 mL). (Note that both superscript 2s
in 2pH/V2 mean second derivative, not squared.) It is desirable to use a
spreadsheet program to carry out the calculations such as Excel, Origin, Sigma
Plot, Igor, etc. Show these graphs to your TA for approval.
3. Calculations:
Before continuing you must have calculated the equivalent weight of your unknown and
carried out the calculation of the pKa. Regarding the equivalent weight, some unknowns
have a few tenths of percent water or other impurities, so exact agreement with the
theoretical value might not occur.
4. Melting Point Determination
You will be using one of these two types of
melting point apparatus:
1- The manual melting point apparatus, Mel-Temp
(fig. 5.1). This apparatus has an electrically heated
aluminum block fitted with a thermometer reading
up to 300oC. The sample is placed between two 18
mm microscope covers, which are placed on the
aluminum block. The temperature is regulated by
means of a variable transformer, and the sample
temperature is observed with the aid of a
magnifying glass. You only need to use a very
small amount of sample in your measurements.
2- The digital melting point apparatus, DigiMelt (fig. 5.2).

DigiMelt incorporates a platinum resistance temperature
detector (RTD) instead of the usual mercury thermometer.
DigiMelts maximum temperature is 260 C. The sample is
placed in a capillary tube sealed at one end. The tube is then
placed in the sample holder. Up to three samples can be run at
the same time. Students can enter a start temperature, a ramp
rate, and a stop temperature and the microprocessor takes care
of the rest. DigiMelt rapidly heats the oven to the programmed
start temperature, then slowly ramps at the specified rate. The
44
student carefully observes the samples with the aid of a magnifier and records the melting
points with a touch of a button.
Depending on what apparatus you are using, either place a very small amount of your unknown
in between two microscope covers, or fill a capillary with around 3 mm height of the unknown.
1- Place the prepared sample in the sample holder of the melting point instrument.
2- Determine the melting point range of your unknown by performing a rapid run.
3- Prepare a new sample and determine the melting point of your unknown according to
the following:
a. Place the prepared sample in the sample holder of the melting point instrument.
b. Start heating rapidly until the temperature is within 10 C of the recorded melting
point for the sample, then heat slowly so that the temperature rises uniformly at a
rate of not more than 2C per minute.
c. Observe the melting process though the magnifying lens.
d. Observe and record the melting point range, from the time the first drop is
observed until all the sample becomes a clear liquid. Usually, our unknowns melt
within a 2-4C range.
Notes: -
The more slowly the temperature is increased through the melting range, the closer
your values will be to the correct range for the purity of your sample.
A fresh sample must be used for each melting point.
Some of the crystals of organic acid might contain solvent of recrystallization or
water of hydration. Do not confuse the loss of solvent or water with melting. This
phenomenon is called sweating and the crystals seem to melt (to an
inexperienced eye!). It usually occurs 5-10 C before the actual melting.
If you need to repeat the experiment on a different time/day try to use the same
melting point apparatus.
5. Mixed melting point

At this point, you should have all the necessary information to identify your unknown.
Compare your pKa, equivalent weight, melting point, and UV spectra you have experimentally
determined for your acid to those reported in the literature (summarized below). Find the best
candidate for your unknown and discuss the reasoning behind your choice with your TA.
If your reasoning is sound, your TA will give you an authentic sample of the candidate you
have chosen for the determination of a mixed melting point to verify your identification.
a. Mix some of the known acid that you obtained from your TA with your unknown in about
a 50:50 ratio. Crush and homogenize the mixture (The more intimately they are mixed,
the better the melting point result will be).
b. Place some of the mixture in between two melting point covers. Record the melting point
range and include data in Table 5.5. If the melting point of the mixture is 10-20 below
that determined for your pure unknown, the two substances are different. If the melting
point of the mixture is the same as that determined for your pure unknown, then the two
substances are identical.
45
Dissociation Constants and Ultraviolet Spectra of Selected Aromatic Acids

Each acid is identified by its systematic name and also by its common or trivial name if
one exists. pKas determined in 50% or 55% ethanol are listed if available, otherwise values for
aqueous solution are given.
For many compounds, two pKas are given. If the acid also contains a basic nitrogen
(aminobenzoic and pyridinecarboxylic acids), the first pK1 refers to dissociation of the
protonated form:
H3N
(+)
CO2H
K1
H3N
()
(+)
CO2
K2
H2N
()
CO2
m-aminobenzoic acid
If the acid also contains a phenolic hydroxyl, the second pK2 refers to the dissociation of
the phenolic proton:
CO2H
()
()
CO2
K1
HO
p-hydroxybenzoic acid
CO2
K2
()
HO
Ultraviolet spectra are reported for the strongest absorption and were obtained in 95%
ethanol.
46
Compound
Formula
2-methoxybenzoic C8H8O3
acid (o-anisic acid)
Molecular
weight
152.15
Melting
point
102
pka in
water
4.08
pka in
ethanol
Structure
O CH3
O
OH
2-methylbenzoic
acid (o-toluic acid)
C8H8O2
136.14
104
3.91
5.70
CH3
O
OH
3-methoxybenzoic
acid (m-anisic
acid)
C8H8O3
152.15
105-106
4.10
H3C O
O
OH
3-methylbenzoic
acid (m-toluic
acid)
C8H8O2
136.14
109
4.27
5.80
H3C
O
OH
C7H6O2
benzoic acid
(benzenecarboxylic
acid)
122.12
C9H8O4
180.16
2-acetoxybenzoic
acid
(acetylsalicylic
acid, aspirin)
123-124.5
4.202
6.1
O
OH
135
2.48
OH
O
O
CH3
3-nitrobenzoic
acid (mnitrobenzoic acid)
C7H5NO4
167.12
141
3.449
4.70
O
O N
O
OH
2-chlorobenzoic
acid (ochlorobenzoic
acid)
C7H5ClO2
156.57
142-143
2.90
5.2
Cl
O
OH
47
2-nitrobenzoic
acid (onitrobenzoic acid)
C7H5NO4
167.12
148
2.179
OH
O
N+ O
-
3-chlorobenzoic
acid (mchlorobenzoic
acid)
C7H5ClO2
156.57
158
3.84
5.40
Cl
O
OH
2,4-dinitrobenzoic C7H4N2O6 212.12

acid
178-180
1.43
O
N O
O
O
N
OH
4-methoxybenzoic C8H8O3
acid (p-anisic acid)
152.15
184
4.50
O
O
OH
H3C
3,5-dinitrobenzoic C7H4N2O6 212.12

acid
209-212
2.82
4.1
O
O N
O
OH
O N
O
benzene-1,2carboxylic acid
(phthalic acid)
C8H6O4
166.13
231 (132
anhydride)
2.950
5.408
O
OH
OH
O
4-nitrobenzoic
acid (pnitrobenzoic acid)
C7H5NO4
4-chlorobenzoic
acid (pchlorobenzoic
acid)
C7H5ClO2
167.12
242-243
3.442
5.14
OH
+
N
O
156.57
243
3.98
O
Cl
OH
48
Dissociation constants of aromatic acids are among the most thoroughly studied properties in
organic chemistry, as they are basic to the Hammett sigma-rho (linear free energy) treatment
of substituent effects. On the other hand the data tend to be widely scattered in the literature, and
values obtained by different workers using different methods do not always agree precisely. All
the values cited above are taken from secondary sources, with preference given to the values
believed to be most reliable. For some acids, literature pKas were found for water solution only,
but the change in pKa with solvent is fairly constant for closely related compounds. Most
carboxylic acids decrease in acidity by about 1.5 pKa units in going from water to 50% ethanol.
The dissociation of benzoic acids in 95% ethanol is so slight that the acid itself is the
principal absorbing species. The slight bathochromic shift observed for non-basic acids in
changing the solvent from ethanol to aqueous acid is thus a solvent effect; as the acid is
converted to its anion while keeping the medium (water) constant, small hypochromic and
hypsochromic shifts occur. Protonation of an amino group or ionization of a hydroxyl group
attached directly to the aromatic chromophore causes much more distinctive changes in the
spectra.
End Point Determination by First and Second Derivatives
End points can be more accurately determined by the method based on first and second
derivatives. (See Harris section 11-5). To accomplish this, about 1 or 2 mL before the
stoichiometric point is expected, dropwise additions of titrant are made as outlined in the
procedure section above. From this data pH/V can be determined, where pH is the pH
change between drops and V is the change in volume (here one drop, ~ 0.05 mL). In the same
way, 2pH/V2 can be calculated, and plots of pH, pH/V, and 2pH/V2 versus volume are
made*. The second derivative curve must intersect the volume axis at the stoichiometric point.
Note: The superscript 2 in expressions like 2pH/V2 and 2pH/V2 refer to the second
derivative (or difference in differences) and not to squaring any term.
49
Date_____________
Student ID #_______________
Section___________
Experiment 5
Purpose:
Data:
M of KOH =
Results:
Results from the second Titration of unknown (#_____)
Mass of unknown =
Volume at half equivalence =
pH at half equivalence =
Volume at equivalence =
pH at equivalence =
Equivalent Weight of unknown (g/mol) =
Attach the table of pH obtained versus volume added and plot a graph of the pH versus
volume. Show on the graph the pH at equivalence and the pH at half equivalence.
Attach a table for the pH/V and 2pH/V2 values and plot the pH/V versus V of KOH
(first derivative) and 2pH/V2 versus V of KOH (second derivative)
50
Table 5.2 Results for Melting Point and Mixed Melting Point
Melting Point of
Unknown Acid (C)
Mixed Melting Point

(C)
Initial
Final
Range
Identity of the unknown: _________________________

Discussion of Results:
51
Literature Melting
Point Value (C)
Experiment 6
Distillation
Objective: The principle objective of this experiment is:
1- To learn the techniques of simple and fractional distillation.
2- To identify the percent composition of an acetone water mixture via fractional
distillation.
Introduction
The space above the surface of a liquid always contains some of the substance in the vapor
(gaseous) state. If the container is an open one, such as a beaker, the molecules of the vapor
escape to the atmosphere to be replaced by other molecules escaping from the liquid. When this
process takes place below the boiling point of the liquid it is called evaporation. If the container
is a closed system as a corked bottle, an equilibrium is reached in which the air space above the
liquid is saturated with molecules of the vapor. The pressure exerted by the vapor in equilibrium
with the liquid is called the vapor pressure of the liquid. The vapor pressure of the liquid is
constant at a given temperature and is not affected by the total pressure. It is a measure of the
tendency of a liquid to pass into the vapor state. It increases as the temperature is raised and
decreases as the temperature is lowered. The boiling point of a liquid is the temperature at which
the vapor pressure becomes equal to the atmospheric pressure. Thus, as the atmospheric pressure
is raised, the boiling point also is raised, and as the atmospheric pressure is lowered, the boiling
point is lowered. If the temperature of a liquid is raised until its vapor pressure becomes equal to
that of the atmosphere, i.e., to the boiling point, and maintained at that temperature, the liquid
will pass entirely into the vapor state. This process is known as vaporization. If the vapor of the
liquid is conducted to another container which is cooled below the boiling point, it will condense
(return to the liquid phase). When a chemist speaks of distillation he/she generally means the
combined process of vaporization followed by condensation. A typical apparatus for simple
distillation is shown in fig. 6.1.
Pure organic compounds distill over a very narrow range of temperature called by chemists the
boiling point (b.p.). Any liquid with a wide boiling or distilling range is impure, although a liquid
with a very narrow, constant, boiling point range is not necessarily a pure one. The reason for
this is that various compounds are affected in different ways by impurities. Some show no
change in boiling point, others display elevated boiling points, and still others show depressed
boiling points. For this reason the boiling point of a substance, while valuable, is not as good a
criterion of purity as is the melting point.
Volatile liquids can be separated from nonvolatile substances by distillation, and, frequently,
mixtures of volatile liquids can be separated into the component parts by fractional distillation.
Occasionally, two or more liquids form a constant-boiling mixture or azeotrope, which boils at a
constant temperature and is made up of a fixed composition of the components. For example,
pure ethyl alcohol boils at 78.4C and pure water at 100C, but a mixture of 95% ethyl alcohol
and 5% water boils at 78.1C, and this mixture cannot be separated by distillation into pure water
and pure ethyl alcohol. Other mixtures having different percentage compositions of ethyl alcohol
and water can be separated by distillation into one of the components and the azeotrope.
52
During distillation a particular portion of the liquid may become momentarily heated above the
boiling point, a large amount of vapor may form suddenly, and the contents of the flask may
bump possibly carrying liquid up through the side-arm of the distilling flask and causing the
apparatus to be jolted severely. Bumping may be prevented to a large extent by adding a few
pieces of porous boiling stones or carborandum. These mineral substances contain considerable
air in their porous structures which act as a source of tiny bubbles, first of air, later of the volatile
components. The vapors of the liquid will form around these bubbles with little local
superheating.
Fig. 6.1 Simple distillation set-up
Fractional Distillation
A mixture of miscible liquids (i.e., each totally soluble in the other but boiling at different
temperatures) may not be totally separated by simple distillation. The first distillate of such a
mixture (called the forerun), although containing some of the higher boiling material, will always
be richer in the lower boiling component. If the initial distillate is redistilled, the first vapor and
condensate again will be richer in the lower boiling component. The process, if repeated a great
many times, will result in a fairly good separation of the mixture. Obviously, this would be a
laborious and time-consuming process. A fractionating column is an ingenious device which
eliminates the necessity for this multiple manipulation. The fractionating column is a vertical
column packed with some inert material such as glass beads, glass helices, clay chips or copper
sponge to provide a large surface upon which vapor can condense. As the hot vapor rises through
this packing it condenses in the cooler part of the column. The condensate flows downward until
it reaches a portion of the column sufficiently hot to reconvert it to vapor. Each time the
condensate vaporizes, the vapor is again richer in the lower boiling component than the
preceding portion, and the residual liquid in the still-pot becomes richer in the higher boiling
53
component. This process, repeated a great number of times in the packed column, finally
produces vapor of the lower boiling component that passes as a pure compound through the sidearm of the column and into the condenser. The lowest boiling component will continue to pass
over at its boiling point until it is almost completely separated from the mixture. The temperature
of the liquid mixture remaining in the flask then will rise to the boiling point of the next lowest
boiling component, and so on until a separation of the liquid mixture is made. This process is
called fractional distillation. Figure 6.2 illustrates a typical fractional distillation apparatus.
Fig. 6.2 Fractional distillation apparatus

If you have a mixture of two liquids, A and B, the total vapor pressure will be equal to the sum
of the two individual partial vapor pressures.
PT PA PB
It is important to note that; the pressure due to component A influences the pressure due to
component B. We really have to think about how much of each component is present. We do
this by considering Raoults Law:
PA XA PAo
54
Where PAo is the vapor pressure of pure A at a particular temperature, and XA is the mole fraction
of A. The partial pressure of A is equal to the mole fraction of A times the vapor pressure of pure
A. At the heart of distillation is the sensible fact that at any given temperature the lower boiling
(more volatile) component of a mixture makes a larger contribution to the vapor composition
than the higher boiling component. In our example, below, A is the lower boiling component.
The vapor, then, is richer in A than the liquid from which it escaped. This is represented
graphically below, fig. 8.3. A 1:1 molar liquid mixture (having composition L1) boils at
temperature T1, where the composition of the vapor is V1 (here, ~ 9:1 mole ratio of A:B).
Condensation of this vapor yields a liquid that has been purified in A to some extent, but B is still
present - how much B depends primarily on the difference in boiling points of A and B. If A is
much more volatile than B, one can often achieve good separation, and a simple distillation will
suffice. However, when A is not much more volatile than B, there will be little enrichment of A.
In this case, one needs to repeat the vaporization-condensation cycle. This can be done by taking
the distillate of the first run and distilling it again (and again); or, one can perform a fractional
distillation.
Fig. 6.3 Liquid-vapor composition diagram of a mixture

Reference: Brewster, Unitized experiments in organic chemistry, 4th Ed.
Procedure
Each student performs a simple distillation and a fractional distillation.
I.
Simple Distillation
1. Obtain around 110 mL of water-acetone mixture of unknown ratio from your
instructor.
55
2. Place 50 mL of the unknown in a 100 mL round-bottomed flask, and add two boiling
stones. Arrange the apparatus as shown in fig 8.1 for simple distillation. Extreme care
should be taken when setting up the distillation apparatus. Side-arms of distillation
flasks and fractionating columns can break easily. Ask your instructor to check the
apparatus.
3. Run a gentle stream of water through the jacket of the condenser. Have ready two
receiving flasks labeled I and II, for collecting fractions. Start heating the distillation
flask using a low flame to allow collection of condensate in flask I at a rate of one
drop a second. Change the receiving flask to that labeled II when the temperature just
exceeds 62C. Collect in flask II the distillate that comes out at temperatures in the
range 62-90C. Then interrupt the distillation, and cool the distillation flask. Measure
the volume of each of the two distillates in receivers I and II and the volume of the
residue in the round bottom flask. Record your measurements as follows:
Fractional I, boiling range: 55-62C, Volume: _________________

Fraction II, boiling range: 62-90C, Volume: _________________
Residue,
Volume: _________________
4. Redistill fraction II and collect the sub-fraction that distills at a temperature of up to

62C, then the fraction that distills between 62-90C. Measure their volumes and add
them to corresponding previously recorded volumes.
5. Evaluate the extent to which the second simple distillation improves the separation of
the two liquids.
II.
Fractional Distillation
Set up the apparatus as shown in figure 6.2 and perform the experiment as described for
the simple distillation. Measure the volume of each of the fractions and the residue.
56
Date_____________
Student ID #_______________
Section___________
Experiment 6
Distillation
Purpose:
Data and calculations:

Table 6.1 Table of Reagents
Compound
Formula
M.Wt.
(g/mol)
Boiling point
(C)
Volume I (mL)
56-62 C
Volume II (mL)
62-90 C
Residue (mL)
Table 6.2 Results

Unknown # = ____
1st Simple
distillation
2nd Simple
distillation
Total volume
Fractional
distillation
(unpacked column)
57
Calculation of % Composition of the Unknown

i-
% of acetone obtained by 1st simple distillation =
ii-
% of acetone obtained by 2nd simple distillation (use total volume) =
iii-
Total % of acetone obtained by simple distillation =
iv-
% of acetone obtained by Fractional distillation =
Ratio of your water-acetone mixture:
Sources of Error:
58
Experiment 7
Recrystallization
1- To select a crystallizing solvent for three different compounds.
2- To crystallize acetanilide and determine the yield and melting point of the pure
product.
Introduction
Organic compounds are usually more soluble in hot solvents than in cold ones. An impure
solid organic compound, when dissolved in the proper amount of an appropriate solvent at an
elevated temperature will reprecipitate when the solution is cooled. If the hot solution is filtered
before being allowed to cool, dirt, lint, or other insoluble impurities will be removed, and the
crystals that deposit in the cooled solution are usually more pure than the starting material is. The
crystals may be removed from filtrate (mother liquor) by filtration. The soluble impurities and a
small amount of the desired substance will stay in solution. This process is called
recrystallization which is frequently used for the purification of solid organic compounds. The
success of the process depends on the fact that soluble impurities usually are present in smaller
amounts than the desired compound so that the cooled solution, although saturated with respect
to the desired product, may not be saturated with the impurity. This being the case, the latter will
not precipitate from the solution. Sometimes a solution does become saturated with respect to an
impurity during the cooling process. In this event, the impurity deposits along with the desired
product and the recrystallization will have to be repeated, perhaps several times. In each
recrystallization, a small amount of the desired compound remains behind in the mother liquor.
Such loses are unavoidable if a pure product is to be obtained.
A good solvent for recrystallization has the following properties: (1) it dissolves a reasonable
amount of the organic compound at high temperatures (usually the boiling point of the solvent)
and very little at low temperature, (2) it dissolves impurities readily at low temperatures or does
not dissolve them at all, (3) it does not react with the substance being purified, (4) it has a low
boiling point so that it is readily removed from the purified product, and (5) it is cheap.
Sometimes a solvent with all of these properties cannot be found. In such instances the solvent
that most nearly approaches the ideal is selected. Alternatively one may use miscible solventpairs.
The process of recrystallization often may be aided, especially when the impurities are colored,
by selectively adsorbing contaminants on activated charcoal (Norit). A small amount of charcoal
is added to the hot solution just before the filtration step. However, charcoal will adsorb not only
the impurities but also a certain amount of the desired product. It is advisable, therefore, to use a
minimum amount of charcoal.
Recrystallization is a process in which you take some crystals, dissolve them in a solvent, and
turn them back into crystals again. As noted above, the purpose is to separate the impurities from
the desired substance. The practical process of recrystallization can be described in seven steps,
as follows (the reason for each step is given in parentheses); First, choose a solvent that doesnt
dissolve the compound when cold, but does when hot, (these properties of the solvent make the
59
recrystallization process possible). Add hot solvent until the compound you are trying to purify
dissolves, (this makes impurities that were locked inside the impure crystals available for
removal). Add decolorizing charcoal if colored impurities are present, (the colored molecules are
adsorbed onto the surface of the charcoal). Filter the resulting solution while it is still hot, fig.
7.1, (this step separates two kinds of impurities from the substance you want). The charcoal with
the colored molecules adhering to them are trapped on the filter paper, and so are particles of
impurities that didnt dissolve in the hot solvent to begin with. Cool the solution and obtain
crystals of your desired compound, (soluble impurities will remain in solution). Perform suction
filtration to isolate the compound, fig. 7.2, (the soluble impurities and most of the
recrystallization solvent are separated from the compound you want in this step). Drying the
crystals youve isolated, (this removes the rest of your recrystallization solvent, which is an
impurity).Here are the setups used for hot filtration and suction filtration.
Hot Filtration: The fluted filter paper in hot filtration has a large surface area, allowing for fast
filtration (before the solvent cools); it traps the charcoal and any insoluble impurities, and lets the
solvent (containing the desired compound and the soluble impurities) go through, (fig. 6.1).
Fig. 7.1 Hot filtration set-up

Suction Filtration: For the collection of the pure crystals suction filtration is applied, employing
especially designed funnels (e. g. Buchner funnel or Hirsch funnel) to effect rapid filtration and
drying of precipitates, (fig. 6.2). Further drying can be effected in an oven at a suitable
temperature.
Fig. 7.2 Set up for suction filtration

60
Procedure
I.
Selection of a crystallizing solvent
Determine the solubility of anthracene, benzoic acid and sodium benzoate in water, toluene and
ligroin (See procedure below). According to the results, select the best crystallization solvent for
each. Record data and observations in Tables 7.1 and 7.2.
1. Transfer, using a spatula, about 0.1 g of the finely divided solid into a test tube
(150*18mm). It is not necessary to use a balance to measure out the solids accurately.
2. Measure in a small graduated cylinder 3 mL of the solvent. Add the solvent onto the solid
dropwise with continuous shaking until a total of one mL is added. Complete dissolution
will leave a clear or transparent solution. The solution may be colored if the solid is
colored.
If the entire solid has dissolved in the 1 mL solvent at room temperature, then the solvent
is unsuitable for crystallization. Therefore nothing more has to be done with that
compound concerning this solvent.
If it is insoluble at room temperature, heat the reaction tube to the boiling point of the
solution using the heating blocks placed on top of the heating plates. Do not forget to
place digital thermometers in the heating blocks to control your temperatures. Start your
tests from the lowest boiling point solvent. If the entire solid dissolves, it can be declared
readily soluble in the hot solvent.
If it is still insoluble after a while of boiling, add more solvent in 0.5mL portions until
all of the solid dissolves at the boiling point or until a total of 3mL of solvent is present
In the cases where the solid dissolved in boiling solvent, allow the tube to cool slowly to
room temperature, undisturbed, scratching the sides of the test tube with a glass rod to
induce crystallization. In these cases, the liquid is a good crystallization solvent.
If some or the entire solid still remains insoluble in the 3mL of the solvent at its boiling
point, then the solvent is unsuitable.
II.
Recrystallization of Acetanilide
Record the required data in Table 7.3.

1. Weigh 1.0 g of crude acetanilide and record data in Table 6.4. Transfer the weighed
acetanilide into a 125 mL Erlenmeyer flask and add 2-3 boiling stones. Add around 10
mL of boiling water.
2. Heat the solution on a hot plate while stirring the flask (with hand) to dissolve the solid.
If the sample does not dissolve when water boils, add more hot water in 2 mL portions
with stirring and heating until the solid dissolves in the boiling water. Note that some
impurities may not be soluble in the solvent and remain undissolved no matter how much
solvent you add. However, make sure that the dark oily material which forms is
61
completely dissolved. Add an additional 5 mL of water at the boiling point and filter the
hot solution through a short stem funnel, which has been previously heated by passing
boiling water through it, into an Erlenmeyer flask. Leave the solution to cool to room
temperature and then in a bath of cold water/ice for 20 minutes.
3. When the solution is cool, collect the crystals by suction filtration and wash with two
separate 3 mL portions of cold water, each time pressing the crystals firmly with an
inverted glass stopper or a cork. Transfer the crystals to a filter paper, and press them
firmly to remove water.
4. Weigh the product and determine its percentage.
5. Determine the melting point of the crude and pure acetanilide and record data in Table
7.5
62
Date_____________
Student ID #_______________
Section___________
Experiment 7
Recrystallization
Purpose:
Data and calculations:

I.
Selection of a crystallizing solvent
Table 7.1 Table of reagents

Compound
Formula
M.Wt.
(g/mol)
Melting point
(C)
Boiling point
(C)
Table 7.2 Results

Compound
Water
Cold Hot
Toluene
Cold Hot
63
Ligroin
Cold Hot
Best solvent for

Recrystallization
Sources of Error:
II.
Recrystallization of Acetanilide

Compound
Formula
M.Wt.
(g/mol)
Melting point
(C)
Boiling point
(C)
Table 7.4 Results

Structure of
Acetanilide
Mass used
(g)
Mass recovered
(g)
% Recovery
Table 7.5 Melting point Determination

Acetanilide
Experimental Melting point (C)
Crude
Pure
Sources of Error:
64
Experiment 8
Chromatography
1- To identify the components of three unknown solutions via TLC
2- To calculate Rf values of the identified unknowns
3- To choose a best mobile phase to run a column for separating the components of a
solution.
4- To purify an impure solution via column chromatography.
5- To separate the components of a dye mixture by column chromatography.
Introduction
Chromatography is a method for the separation of a mixture, based on differences between
compounds in their partitioning between a stationary adsorbent and a moving solvent or carrier.
The adsorbent is described as the stationary phase and the carrier as the mobile phase. A
particular kind of chromatography depends on the types of the stationary and the mobile phases.
In thin layer chromatography (TLC) the stationary phase is a solid, usually powdered silica gel
(SiO2), coated as a thin layer on a sheet of glass or special plates. Some of the chief uses of TLC
include determination of the number of components in a sample, detection of a compound in a
mixture and the identification of an unknown compound by comparison with known compounds.
Since tiny amounts of mixtures are usually applied to the plates and the material is exposed on
the surface of the plates, the use of TLC is essentially limited to non-volatile solids.
The sample to be examined is applied with a narrow capillary as a spot near the bottom of the
slide, (fig. 7.1b). The slide is then lowered into a bottle or a jar that has an appropriate amount of
solvent covering its inside bottom. The solvent is allowed to climb up the slide carrying with it
the components of the mixture at different speeds. When the solvent front is within 1 cm from
the top of the slide, the slide is then removed and the level of the solvent is marked, (fig. 8.1c).
When the slide gets dry from the solvent the position of the various compounds on the slide are
located as spots recognized visually if the substances are colored or by suitable sprays or
exposure to iodine or by UV light. The relative migratabilities of the components of the mixture
are measured by calculating the Rf values:
Rf =
dis tan ce travelled by the subs tan ce

dis tan ce travelled by the solvent
Rf (for spot A) = a/c
Rf (for spot B) = b/c
In general, a less polar or more soluble compound will have a higher Rf value (such as B), than a
more polar or less soluble compound (such as A).
65
a
Spot A
a
B
b
Figure 8.1 a) A TLC sheet; b) The TLC sheet after spotting the samples; c) The TLC sheet
after running it in the solvent; d) distances needed to calculate Rf of each compound.
In column chromatography, the stationary phase, a solid adsorbent, is placed in a vertical glass
(usually) column and the mobile phase, a liquid, is added to the top and flows down through the
column (by either gravity or external pressure). Column chromatography is generally used as a
purification technique: it isolates desired compounds from a mixture (liquids or solids).
The mixture to be analyzed by column chromatrography is applied to the top of the column.
The liquid solvent (the eluent) is passed through the column by gravity or by the application of
air pressure. The equilibrium is established between the solute adsorbed on the adsorbent and the
eluting solvent flowing down through the column. Because the different components in the
mixture have different interactions with the stationary and mobile phases, they will be carried
along with the mobile phase to varying degrees and a separation will be achieved. The individual
components, or elutants, are collected as the solvent drips from the bottom of the column.
Column chromatography is separated into two categories, depending on how the solvent flows
down the column. If the solvent is allowed to flow down the column by gravity, or percolation, it
is called gravity column chromatography. If the solvent is forced down the column by positive
air pressure, it is called flash chromatography.
In this experiment you will identify an unknown by TLC and you will separate a dye mixture
into is components by column chromatography.
66
Procedure (Work in pairs)

I.
1.
2.
3.
4.
5.
6.
7.
8.
9.
Thin Layer Chromatography for the Unknowns

Obtain a TLC plate, a capillary tube and three colored solution samples which are
numbered.
Record the numbers of the vials in your report. The colored samples can either be onitroaniline, or p-nitroaniline and a mixture of both which you have to identify at the
end of the experiment.
Prepare a TLC plate for the three solutions according to the following procedure:
a. Using a pencil, draw two light marks at each side of the plate about 1 cm from the
bottom and the top. Make sure you do not scratch the silica when you draw the
line on the plate.
b. Draw 3 very small circles on the line about 0.5 cm from the sides of the TLC plate
and from each other. Label the circles with the solutions you want to test.
c. Fill your capillary with the desired solution and carefully touch it vertically to the
TLC plate at the corresponding spot. Do not put down the entire contents of your
capillary at once. Rather, spot, allow the spot to dry, and spot again at the same
place. You will observe a colored spot.
d. Keep spotting until the color of the spot is intense. (You may only need to spot
once if your solution is concentrated).
e. Spot the other solutions similarly at the corresponding position using a new
capillary.
Fill a 400 or 600 mL beaker with hexane, to a height of not more than 3-4 mm.
Place a filter paper on the inner wall of the beaker and wet it with the solvent.
Place your TLC plate in the beaker and cover the beaker with a watch glass or an
aluminum foil.
Wait until the solvent front is 1 cm from the top of the covered part of the plate or until
it reaches the marked line.
Remove the slide, mark lightly the solvent front, locate the position of each substance
and calculate its Rf value, (fig. 8.1.d).
Repeat the same procedure with two different solvents, hexane:ethyl acetate (90:10),
and ethyl acetate.
N.B: To save time, you can first prepare the three TLC plates, then the three beakers (each with a
different solvent) and finally run the three at the same time.
10. Determine the best mobile phase to use for column
chromatography.
11. Determine which vial contains one compound and
which contains a mixture of two compounds.
12. Identify the composition of the component/s in each
vial.
67
II.
Column Chromatography Procedure for the Impure

Solution:
1. Obtain a clean and dry buret from your instructor.
2. Place a piece of glass wool at the bottom.
3. Add 0.2 cm of sand on top of the cotton in an even way.
4. Weigh around 8 g of silica (around 10 cm graduation)
and add it on top of the sand in portions with tapping of
the buret after every addition to ensure good packing.
5. Add 0.2 cm of sand to the top.
6. Connect the column to a secured suction filtration flask
and apply vacuum (see figure 7.2).
7. Pre-elute the column by adding hexane to the top of the
column (around 6 mL), opening the stopcock to let the
solvent move to the bottom.
8. When solvent starts to exit the column, let the eluting
solvent drain to approximately 0.5 cm above the top of
the sand (always collect the solution coming out of the
buret with an Erlenmeyer flask or a beaker and never let your column run dry), then
close your stopcock.
9. Detach the hose and transfer 0.5 mL of your impure solution into the column.
10. Drain to approximately 0.5 cm above the top of the sand by suction.
11. Add around 2 mL of the mobile phase (identified previously as the best for column
chromatography) and drain until the solvent level (in the column) is approximately 0.5
cm above the sand.
12. Repeat the former step until you do not observe any coloring of the solvent when
added on top of the sand; then start adding large volumes of the elution solvent on top
of the sand and elute. What you will notice as the solvent is moving down the column
is the separation of two bands.
13. Collect the first band (around a total of around 50 mL of solvent to elute the first
band). Under these conditions, the ortho isomer will elute from the column first and
the unwanted para isomer will remain on the column.
14. After collecting the first band, the ortho, close the stopcock, stop the suction, detach
the flask from the buret, transfer the collected ortho isomer to an Erlenmeyer flask,
clean your suction flask with acetone and then connect the flask back to the buret to
continue.
15. Drain the mobile phase to reach a level of approximately 0.5 cm above the sand before
adding the next mobile phase to collect the second band (need around 15 mL).
16. Collect the second band using the proper mobile phase.
Note: In case some water entered your suction flask while performing column chromatography,
you will observe two layers in the suction flask. In this case, transfer the solution to a separatory
flask, collect (in an Erlenmeyer flask) the lower layer from the bottom of the flask, while the top
layer, the needed layer, from the top of flask into a different flask than the one used for collecting
the lower layer. To be sure which layer is the aqueous, add water to the solution in the separatory
funnel. The layer that gets larger is the aqueous.
68
III.
Column Chromatography for the Dye Mixture (demonstration):
You will be using one of these solutions:
a- Mixture of Fluorescein and methylene blue (1.7 mL)
b- Mixture of methyl orange and methylene blue (1 mL)
c- Mixture of methyl orange and victoria blue (1 mL)
Obtain a clean and dry buret. Place a piece of glass wool at the bottom and add 0.2 cm of sand on
top of the cotton in an even way.
1- Weigh around 10 g of activated adsorption alumina and 0.7g of Hyflo Super-cel. Mix them
well in a beaker and add it on top of the sand in portions with tapping of the buret after every
addition to ensure good packing. Add 0.2 cm of sand to the top.
2- Connect the column to a clamped suction flask and apply vacuum.
3- Pre-elute the column by adding ethanol to the top of the column (around 10 mL) and
opening the stopcock to let the solvent move to the bottom. When solvent starts to exit the
column, let the eluting solvent drain to approximately 0.5 cm above the top of the sand and
then close your stopcock and detach the hose.
4- Transfer the specified amount of your assigned dye into the column. Drain to approximately
0.5 cm above the top of the sand by suction. Add around 2 mL of the mobile phase and drain
until the solvent level (in the column) is approximately 0.5 cm above the sand. Repeat the
former step until you do not observe any coloring of the solvent when added on top of the
sand; then start adding large volumes of ethanol (the elution solvent) on top of the sand and
elute.
5- What you will notice as the solvent is moving down the column is the separation of two
bands. Collect the first band and identify it.
6- After collecting the first band, stop the suction, detach the flask from the buret, transfer the
collected dye to an Erlenmeyer flask, clean your suction flask with acetone and then connect
the flask back to the buret to continue.
7- Drain the mobile phase to reach a level of approximately 0.5 cm above the sand before
adding the next mobile phase to collect the second band. Add water as the mobile phase and
elute your second band and identify it.
8- Record the observations in Table 8.6.
69
Date_____________
Student ID #_______________
Section___________
Experiment 8
Chromatography
Purpose:
Data and Calculations:

Compound
Formula
M.Wt.
(g/mol)
70
Melting point
(C)
Boiling point
(C)
Results:
I.
TLC:
Unknown #: ________
Table 8.2 Plate # 1 in hexane
Compound
# of
spots
D solvent
(cm)
D compound 1
(cm)
D compound 2
(cm)
Rf 1
Rf 2
D compound 2
(cm)
Rf 1
Rf 2
D compound 2
(cm)
Rf 1
Rf 2
Table 8.3 Plate # 2 in hexane: ethyl acetate (90:10)

Compound
# of
spots
D solvent
(cm)
D compound 1
(cm)
Table 8.4 Plate # 3 in ethyl acetate

Compound
# of
spots
D solvent
(cm)
D compound 1
(cm)
a-Which solvent is the best to separate your components in the mixture? Explain.
b-Identify the composition of the component(s) in your three unknowns
71
Sources of Error:
II.
Column Chromatography:
Table 8.5 Column chromatography data for the impure solution

Vial # _____
# of
spots
D solvent
(cm)
D compound
(cm)
Rf
Fraction 1
a- Is the collected fraction pure? Explain briefly
b- Identify the compound in the collected fractions by comparing the location of the
spots in the collected fraction to those of the pure solutions (in the vials)
Sources of Error:
72
Table 8.6 Data for elution of dyes

Mixture
First eluted
component
Second eluted
component
Sources of Error:
73
Conclusion
Experiment 9
Objective: The objective of this experiment is to synthesize isoamyl acetate.
Introduction
Esters usually have characteristic flavors and fragrances. An odor is detected when a molecule
fits into an olfactory receptor site for that odor and activates it. The molecules functional
groups, size and three dimensional shape are defining criteria for whether the substance has a
specific odor.
O
O
O
O
Isoamyl acetate
Banana
(Alarm pheromone of honeybee)
O
Octyl acetate
Oranges
Propyl acetate
Pear
O
O
Isobutyl propionate
Rum
Ethyl butyrate
Pineapple
Methyl butyrate
Apple
O
O
O
O
OH
O
Ethyl phenylacetate
Honey
Methyl Salicylate
Oil of Wintergreen
Benzyl acetate
Peach
The synthesis of isoamyl acetate, sometimes called banana oil, illustrates the acid catalyzed
esterfication process:
CH3
O
CH3COH
H2SO4
HOCH2CH2CH
O
CH3COCH2CH2CH
CH3
+
H2O
CH3
CH3
The esterfication reaction involves an equilibrium that is attained only very slowly when the
organic acid is allowed to react with the alcohol in the absence of a catalyst. The addition of a
strong mineral acid such as sulfuric or hydrochloric acid, while catalyzing the reaction greatly,
does not affect the position of the equilibrium. To force the reaction to the right (i.e., to increase
the amount of ester formed), two steps can be taken: (1) either reactant (usually the less costly)
74
may be used in excess of the amount called for by the reaction equation, or (2) either of the
products may be removed as it is produced. This experiment deals with the preparation of a
typical ester, isomyl acetate. Isomyl acetate (b.p. 142760) is a relatively common organic solvent
used in paints, and lacquers.
Procedure
1. Obtain form the instructor 17.6 g (22 mL, 0.2 mole) of isoamyl alcohol (d = 0.81 g/mL)
and transfer it to a 100 mL round-bottomed flask
2. Add 30 g (30 mL, 0.5 mole) of glacial acetic acid (d = 1.01 g/mL) and, very carefully, 1
mL of concentrated sulfuric acid.
3. Swirl the flask gently to thoroughly mix the reactants, add two boiling chips and
assemble a reflux apparatus as shown in the figure following.
4. Start the water flowing through the condenser and heat the mixture to boiling over a low
flame.
5. Allow the reaction mixture to reflux for one hour.
6. Cool the solution in the reaction flask by immersing it in a cold water bath and then pour
it into 100 mL of cold water contained in a 400 mL beaker.
7. Transfer the mixture into a separatory funnel and run off the aqueous layer which
contains most of the unreacted acetic acid.
8. Add to the organic layer in the separatory funnel a saturated solution of sodium carbonate
very slowly until the mixture is slightly basic (use litmus paper).
9. Discard the aqueous layer.
10. Wash the crude ester with 30 mL of water, by adding the water to the ester in the
separatory funnel and shaking the mixture for several minutes.
11. If an emulsion is obtained, add approximately 0.2 g of sodium chloride and shake.
12. Separate the layers and discard the aqueous layer.
75
13. Transfer the ester to a 50 mL Erlenmeyer flask and dry it with anhydrous magnesium
sulfate.
14. Filter the liquid into a 125mL erlenmeyer flask (previously pre-weighed by the instructor)
through a long-stemmed funnel fitted with a small plug of cotton.
15. Submit your product to your instructor and obtain its mass.
76
Date_____________
Student ID #_______________
Section___________
Experiment 9
Purpose:
Table of Reagents/Products:
Compound
Formula
M.Wt.
(g/mol)
Mass
(g)
Volume
(mL)
Melting
point
(C)
Boiling
point
(C)
# of
moles
Results:
Limiting Reactant
Exp. Yield
(g)
Theo. Yield (g)
77
% yield
Sample Calculation:
Purification Steps:
78
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Department of Chemistry

Introduction to Chemical Analysis Lab.

A few tips to make life a little easier in Analytical

Locker equipment list

Measuring the Density of Water

Preparation of Primary Standard solutions and

Determining Iron Content in Foods by

Synthesis of Isoamyl Acetate

Periodic Table of the Elements

Safety Rules by the Environmental Health, Safety,

Pour water into acid

Environmental Health, Safety,

If the spill is in a corridor or other public passageway:

Common Laboratory Equipment

A few tips to make life a little easier in

Using the Analytical Balance

Using a Glass Buret

So the average is 0.319 with an average deviation of 0.002.

2 Beakers, glass, 100 ml

2 Beakers, glass, 150 ml

2 Beakers, glass, 250 ml

1 Beakers, glass, 400 ml

1 Beakers, glass, 600 ml

1 Cylinder, graduated, 100 ml

4 Flasks, erlenmeyer, 250 ml

1 Flask , erlenmeyer, 500 ml

6 Flasks, volumetric, 100 ml

Student Imail:_____________ Locker No: ________

Lab Sec.:_________ Day: _______

I have received one desk key and the above items

There are a variety of ways to calculate standard deviation.

Comparing the Measuring Accuracy of Different Volumetric Glassware.

Measuring the Density of Water

B. Data and Calculation:

Comparing the Measuring Accuracy of Different Volumetric Glassware

Mean density = _________________________

Mean density = _________________________

Mean density = _________________________

3. What does standard deviation measure?

(b) What is the source of random error in your measurements?

(c) Did your measurements exhibit systematic error? Briefly explain.

Determining the Density of an Unknown Solution

Unknown number: ______________

Data and calculation:

Mean density for the unknown = _________________________

Standardization of HCl with Na2CO3

Determining the Concentration of an Unknown Na2CO3 Solution

Reference: Harris, Quantitative Chemical Analysis, 7th Ed.

Preparation of Primary Standard Solutions and

Preparation of the primary standard Na2CO3

Table 2.I: Data and calculation of the concentration of Na2CO3

Standardization of the HCl Solution

Volume of Na2CO3 aliquot =_________________

Determining the Concentration of an Unknown Na2CO3 Solution

V HCl (average) = _______________________

CO32- (aq) + 2H+(aq)

Preparation of the Unknown

Total Alkalinity Determination:

Bicarbonate Content Determination

Analysis of a Mixture of Carbonate and Bicarbonate

Data and calculation:

Table 3.2 Total alkalinity determination

Upper buret reading

Student Imail:_____ Locker No:

Lab Sec.:___ Day: _