University of Mines and Technology (UMaT)

Department of Chemical and Petrochemical Engineering

Analytical Chemistry Laboratory Practices

Lab Manual for Petroleum Geosciences and Engineering L100

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Contents
EXPERIMENT 1 ............................................................................................................................................... 6
CALIBRATION OF A PIPETTE ........................................................................................................................... 6
EXPERIMENT 2 ............................................................................................................................................... 9
ACID-BASE TITRATION .................................................................................................................................... 9
EXPERIMENT 3 ............................................................................................................................................. 11
DETERMINATION OF WATER HARDNESS BY COMPLEXOMETRIC TITRATION............................................... 11
EXPERIMENT 4 ............................................................................................................................................. 14
GRAVIMETRIC ANALYSIS OF SOLUBLE CHLORIDE......................................................................................... 14
EXPERIMENT 5 ............................................................................................................................................. 16
pH AND BUFFER SOLUTIONS ....................................................................................................................... 16

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Most of the laboratory safety rules are based on common sense. In the midst of completing a lab
section, however, you may not remember to follow your common sense. Remember the most
important lab safety rule is to be aware of what is going on around you.

RULES
• Wear your eye shield (goggles or an approved protective glasses) at all times in the lab. Do
not wear your contact lenses. Get a pair of goggles that are comfortable.
• Wear shoes in the lab. Bare feet and open-toed shoes are prohibited to prevent dangers from
dropped glassware.
• Confine long hair and loose clothing (scarves and ties) in the lab. Get yourself a lab coat to
use in the lab if you like your clothes. A lab coat also provide an extra layer of protection.
• For handling hazardous chemicals, wear the correct protective equipment (lab coat, apron
neoprene gloves, face shield).
• Do not perform unauthorized experiments. Use only the quantities and types of chemical
listed in the lab.
• No eating or drinking in the laboratory. This applies to food and chemicals. No
mouthpipetting- always use a pipette bulb.
• Do not touch chemicals. Many hazardous chemicals are absorbed through the skin. Wash
off all chemicals that contacts your skin inadvertently with a large amount of water. Do not
dispose of chemicals (any chemicals) through the sink drain. Chemicals are collected in
aqueous or organic collection bottle. Always ask your TA.
• That said, for some innocuous regents, we may dispose by flushing small quantities down
the sink with running water (DILUTE). ALWAYS ASK THE TA
• Learn the hazards of the chemicals we will be using by Consulting the material safety data
sheets.
• Never work alone in the laboratory. There must be at least one other person in the room.
Also, the instructor or TA should be quickly available

EMERGENCIES
• Read emergency directions posted near the door on the red paper. In the event of a serious
emergency; (1) Notify Occupants, (2) Evacuate and (3) Call 911.
• In case of fire or accident, call the instructor or TA immediately. No accident is too small or
too embarrassing to handle it on your own.
• If you or your clothing catches on fire, DO NOT RUN. Do not run. Get somebody to get
the fire blanket and wrap you. Once wrapped, drop to the floor and roll to extinguish the
flames. If you were alone or near the emergency shower, use the emergency shower to do
away with the flames.
• Know the locations of the fire extinguishers: (1) near the fume hood and (2) near the door.
• If you get a chemical in your eyes, wash with flowing water for the eyewash sink for at least
15 minutes. Get somebody to help you keep your eyes open. Get medical attention
immediately.

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• If you spill chemicals on your body or clothing , wash the affected area with a large
amount of water . Use the emergency shower. Get somebody to help you . Remove
clothing affected by the spill to prevent further reaction.
• Know the location of the emergency shower and eyewash sink.
• Report all injuries, even superficial ones, to the instructor or TA immediately. You may not
be aware of the dangers of open wounds in the presence of chemicals used in the lab . Use
the first aid kit in the lab if necessary . If the injury requires medical attention , the instructor
or TA will take you to Health Centre.

ADVICE
• Be responsible for your safety and the safety of those around you . The dangers of spilled
acids and broken glassware are real.
• Avoid breathing fumes of any kind. To test the smell of a vapour, use your hands to waft is
towards your n ose. Work in a fume hood if noxious or poiso nous v apour may be present.
• Keep your work area neat at all times. Clutter slows your work and leads to accidents. At
the end of lab, clean up your area.
• Be careful when heating liquids . Never use an open flame (e.g., Bunsen burner) in this lab.
• Always pour acids into water when mixing . If you pour water into acid , the water
dissociates violently (H2O = H+ + OH-) and the acid will splatter. Remember, “acid into
water is the way that you oughter”.
• Do not force glass stoppers out of ground-glass bottles. Do not force rubber stoppers onto
thermometers or glass tubing. For ground-glass joints, (1) tap the joint, (2) allow water to
wet the joint, and (3) Dissolve the solid that precipitates in the joint (try Coca-Cola). For
thermometers, lubricate and protect your hands.
• Be prepared for the lab if you haven't read the lab , you‟ll miss information about
potentially hazardous chemicals. You will be a hazard to everybody in the room. You‟ll
probably take longer to finish the lab and you won't learn as much as the p roperly
prepared students.

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 LABORATORY REPORT
Your Lab report is a typewritten, lengthier version of the lab notebook in paragraph form (no
outline), and should include the sections below,

1. Title page- write the title of the experiment, the name of the experiment(s) and dates of the
experiments (5 points)
2. Introduction or Background (20 points)
Answer or include the following
• What was the experiment all about? (i.e. state the purpose of the experiment). What
was analyzed and using what method?
• Briefly describe the theory involved (this depends on the methods used).
• Include pertinent chemical equations
3. Procedure (15 points) – using your own words
• Write a summary of the procedure that was followed during the experiment in
paragraph (Remember to use past tense).
• Include all the instrumental parameters used, if applicable.
• For very lengthy procedures, you may simply cite the reference but a brief
descriptions of the steps followed.
4. Data (30 points)
• Tabulate your data. Give an appropriate title and number (Ex Table 1-1)
• Include figures (with appropriate figure title and number) and sample calculations,
if applicable
5. Results and discussions (25 points)
• Discuss your results, including any trends or new findings and their relevance.
• Answer the objectives of the experiment.
• Discuss sources of errors.
• Suggest ways of improving the experiment, if applicable.
6. References (5 points)
Author, title of book or journal, edition (if applicable), City published (for books),
Publisher, Year of publication.

Since the write up is based on a work that has been completed, you must use the past
progressive tense, and do not use pronouns like „I‟ or “We”. For example do not say “I
will prepare 250 mL of 0.01 M NaCl solution instead say “A 250 mL solution of 0.01 M
NaCl was prepared.”

YOU WILL BE GRADED BY THE ABOVE FORMAT THANK YOU

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 EXPERIMENT 1
CALIBRATION OF A PIPETTE

Introduction:
Whenever a measurement is made in the chemistry laboratory some uncertainty exists. It is
desirable to keep this uncertainty as small as possible and obtain measurements that are but precise
and accurate. Precision in the laboratory implies that when a series of measurements are taken that
they will be closed in value to each other. When measurements of an object are accurate, they are
close to the true value of that object. Ideally, our laboratory glassware and instruments will always
be both accurate and as precise as possible.

In this experiment, you will determine the accuracy of a pipette. Pipettes are commonly used in the
laboratory to quickly measure or transfer small amounts of liquid. Many pipettes are labelled with
the uncertainty of the pipette. The true volume of the pipettes will be determined indirectly from
the mass of a sample of distilled water in the known density of the water using the equation, D=M/V,
the volume of the pipettes that may be found from the other two variables. An analytical balance
and a list of densities of water at given temperatures will allow you to determine the volume to four
significant digits. This procedure will be repeated to give some indication of the precision of your
measurement. Once the volume of the pipette has been determined, the pipette will be used to
measure the density of an unknown liquid.

Purpose:
The purpose of this experiment is to calibrate a pipette and to use this pipette to determine the
density of an unknown.

Equipment/Materials
Pipette Pipette bulb
Analytical balance Kim wipes (tissue paper)
Vial, small Beaker, or flask Unknown liquid

Safety:
• An apron and goggles should always be worn in the lab.
• Never draw a liquid into a pipet by mouth. Use a pipette bulb.
• The balances are delicate instruments and should be treated with care.

Procedures:
1. It is necessary to determine the true volume of the pipette you will use in this experiment.
To calibrate your pipette, weigh a small, clean flask or beaker as accurately as possible.
Record the mass of the container on the data sheet.
2. Carefully fill the pipette, adjust the water to the line , and transfer the contents to the
container. The last bit of water should be removed from the pipette. Weigh the container
and the water. Record the value on the data sheet.

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 3. Repeat the procedure four more times.
4. Since the density of water varies with temperature, measure the temperature of the water
that you used . Refer to the following table to find the density of the water . Record the
value in the data table.

Temp 0C Density g/mL Temp. 0C Density g/mL

18 0.9986 22 0.9978
19 0.9984 23 0.9976
20 0.9982 24 0.9973
21 0.9980 25 0.9971

5. Using the mass of water in the sample and the density of the sample, calculate the volume
of the sample and thus the volume of the pipette.
6. What is the average amount held from your determinations? Calculate the standard
deviation of your measurements
7. What is the percent relative error in the 10ml specification of the pipette? Is this within
specifications listed on the pipette?
8. What was your precision in determining the volume of your pipette by this method? Express
as relative standard deviation in parts per thousand.

Data:

Calibration of the pipet

Trial 1 Trial 2 Trial 3
Mass of container & water
Mass of empty container
Mass of water
Temp. of water
Volume of water
True volume of pipette

Average value for volume of pipette_______________. (Use this value for future calculation)

Post Lab Question

1. Sammy Erhead applied for a job last summer in the quality control lab of the Acme Pill
Company. The job was to determine the amount of aspirin in aspirin tablets. He was given
twelve samples of known aspirin content (325 mg) to analyze during his training session.
He completed four sets of trials with three samples in each trial. Which sets had results that
were:

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 a. precise and accurate?
b. precise but not accurate?
c. not precise but accurate?
d. Neither precise no accurate?

Set A Set B Set C Set D

325 mg 300 mg 400 mg 250 mg
325 mg 325 mg 400 mg 280 mg
325 mg 350 mg 400 mg 350 mg

PS- Sammy spent the remainder of the summer sweeping floors at the factory. Good technique is
important.

2. A student completes this experiment using a dirty pipette. He does not notice that several
drops of liquid remain in the pipette each time it is used. How would this affect the
determination of the volume of the pipette?

3. How would this experiment be affected if the balance gives masses that are 20 mg higher
than the true masses every time it is used?

4. What are some things that could have been done to increase the accuracy and precision of
your determination of the volume of the pipette?

5. From the table of density versus temperature of water below, find the appropriate density
and calculate the actual volume of water in your pipette. Then answer the following
questions:
a. What is the average amount water held from the three determinations?
Calculate the standard deviation of your measurement.
b. What is the percent relative error in the (25) 10.00 ml specification of the pipette? Is this
within specifications listed on the pipette?
c. What was your precision in determining the volume of your pipette by this method? Express
as relative standard deviation in parts per thousand.

RELEVANT INFORMATION

Common errors that occur in pipetting are:

• Warming of the pipettes by holding the bulb portion in your hand.
• Failure to allow sufficient drainage time.
• Disturbing the residue that should remain in the tip.

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 •
General carelessness in handling the weighing container.
•
Loss of water as you move from eye level to the weighing bottle (sudden
movements will make some water squirt from the tip, slanting the pipette toward
the horizontal before moving reduces this).
EXPERIMENT 2

ACID-BASE TITRATION
Purpose: the purpose of this lab is to experimentally determine the concentration of an unknown
base solution.

This experiment consists of four separate parts.

Part 1: Preparation of an unknown base solution of NaOH.
Part 2: Standardization of the unknown base solution
Part 3: Titration of a base from Part 2 with an unknown acid to experimentally find the exact
concentration of the acid solution.
Part 4: Using the acid solution from Part 3, experimentally determine the unknown base
concentration.
Part 1: Preparation of a NaOH solution of known concentration
a. Weigh out 10-12 tablets into 100 mL beaker. Record the exact mass to two decimal places.
b. Dissolve the solid sodium hydroxide with a small amount of distilled water. Transfer the
solution into a 250 mL volumetric flask and top up to the mark. Heat would be released as
the solid dissolves.
c. Stopper and label this flask with your name. This is your unknown NaOH solution (do not
lose it. Do not spill it).

Part 1 Data:

Mass of NaOH used: ___________________g

Molecular mass of NaOH: _______________g/mole
Volume of water used: ________________mL = ______L

Part 1 Calculations:

Mole of NaOH used: __________moles

Estimated molarity of unknown NaOH base solution = _____mole/L

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Part 2: Determining the exact molarity of your unknown base by titration.
a. Weight out 0.75- 1.00 grams of dry acid. (please record the mass accurately)
b. Clean a 250 ml. Erlenmeyer flask and dissolve this dry acid in 10-15 ml of distilled water.
c. Add 1 mL of bromothymol blue indicator solution to the Erlenmeyer flask.
d. Following the burette filling procedure, load your burette with unknown base solution.
e. Repeat this at least two more times.

Part 2
Data:
Name of dry acid: __________________________________
Molecular mass of dry acid used ________g/mol

Trial # 1 2 3
Mass of dry acid used (grams)
Volume of base used (mL)

The equation of reaction between the dry acid and the sodium hydroxide is:

Part 2 Calculation:
Using the reaction from above, determine the molarity of the unknown base.
Trial # 1 2 3
Moles of dry acid used (moles)
Moles of unknown base used (moles)
Molarity of unknown base (mol/L)
Average molarity (mol/L)

The average molarity you calculated is the exact molarity of the NaOH solution. It is standardized.
Write the average molarity on the flask. Store it away safely, as you will need it in part 3.

Part 3: Standardizing an acid solution by titration.

We will use the standard bottles supplied in the lab. The bottles have various molarities written on
them and this is normally good enough for everyone else.

Procedure:
a. Fill your burette with your base solution from part 2.
b. Prepare a 0.1M HCI Solution
c. Pipette 10ml of the acid into a 250ml Erlenmeyer flask

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 d. Add few drops phenolthalein indicator to the Erlenmeyer flask
e. Obtain a 100 or 250 mL Erlenmeyer flask, rinse it with distilled water to make sure clean
f. Titrate this unknown acid your known standardized NaOH solution
g. Repeat this titration at least twice more.

Data Table
Trial # 1 2 3
mL‟s of HCL used
mL‟s of NaOH used
Calculations: Using MaVaCa=MbVbCb, Calculate the molarity of the acid.

EXPERIMENT 3
DETERMINATION OF WATER HARDNESS BY COMPLEXOMETRIC TITRATION

Hard water
Hard water is due to metal ions (minerals) that are dissolved in the ground water. These minerals
include Ca2+, Mg2+, Fe3+, SO42, and HCO3-. Hardness in our water is due to rain moving through
the vast amount of limestone (CaCO3) that occurs in our area. This is why we measure hardness
in terms of CaCO3; the concentration of the Ca2+ ions is greater than the concentration of any other
metal ion in our water.

Why be concerned with hard water?

The determination of water hardness is a useful test that provides a measure of quality of water for
households and industrial uses. Originally, water hardness was defined as the measure of the
capacity of the water to precipitate soap. Hard water is not a health hazard. People regularly take
calcium supplements. Drinking hard water contributes a small amount of calcium and magnesium
towards the total human dietary needs of calcium and magnesium.
Hard water does cause soap scam, clog pipes and clog boilers. Soap scam is formed when the
calcium ion binds the soap. This causes an insoluble compound that precipitates to form the scam
you see. Soap actually softens hard water by removing the Ca2+ ions from the water. When hard
water is heated, CaCO3, precipitates out. The precipitate then clogs pipes and industrial boilers.
This leads to malfunction or damage and is expensive to remove.

Water Softeners
If you have hard water, you may use water softener to remove the hardness. Salt is mixed with
water to soften it. The Na+ ion from the salt replaces the Ca2+ion but this causes the water to be
too salty for drinking. Water that has been softened should be used only for laundry and bathing.

Types of Hardness
There are two types of water hardness, temporary and permanent.

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Temporary hardness is due to the bicarbonate ion, HCO3, being present in the water. This type of
hardness can be removed by boiling the water to expel the CO2, as indicated by the following
equation.

HCO3 H2O + CO2(g)

Bicarbonate hardness is classified as temporary hardness.

Permanent hardness is due to the presence of the ions Ca2+, Mg2+ , Fe3+, and SO42-. This type of
hardness cannot be eliminated by boiling. The water with this type of hardness is said to be
permanently hard.

How hard is the water?

The degree of hardness of the water is classified in terms of its calcium carbonate concentration as
follows:
Hardness rating Concentration of Calcium Concentration of Calcium
Carbonate (mg/L) Carbonate (g/US gallons)
Soft 0 to < 75 0 to < 5.2
Medium hard 70 to < 150 5.2 to < 10.5
Hard 150 to < 300 10.5 to < 21
Very hard 300 and greater 21 and greater

Complexometric titration
Permanent hardness is usually determined by titrating it with a standard solution of
ethylenediamminetetra acetic acid, EDTA. The EDTA is a complexing, or chelating agent used to
capture the metal ions. This causes the water to become softened, but the metal ions are not
removed from the water. EDTA simply bind the metal ions to it very tightly.
EDTA
EDTA is a versatile chelating agent. A chelating agent is a substance whose molecules can form
several bonds to a single metal ion. Chelating agents are multi-dentate ligands. A ligand is a
substance that binds with metal ions to form a complex ion. Multidentate ligands are many
clawed; holding onto the metal ions to form a very stable complex. EDTA can form four or six
bond with a metal ion.

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EDTA is frequently used in soaps and detergents, because it forms complexes with calcium and
magnesium ions. These ions which are in hard water are bound to the EDTA and cannot interfere
with the cleaning action of soaps or detergents. EDTA is used to remove metal ions from enzymes
that cause food spoilage. It is also used to promote colour retention foods.
Total Permanent Hardness
In this lab, you will be asked to determine the total permanent hardness. EDTA grabs all the metal
ions in the water; not just the Ca2+ ions. This gives us a value that is not truly the concentration of
Ca2+ ions. This causes an experimental error of about 1 % which is acceptable due to the” fuzzy”
endpoints in this type of titration.

EDTA Endpoint colour change

Eriochrome Black T indicator is used in this titration. When it is a chelated or acidified, it produces
a PINK RED solution. When it is not chelated and under basic conditions, it is BLUE.

Sample Problem
You are using EDTA with a molarity of 0.0080 for the titration. You titrate 50.00 mL of water
sample using 10.68mL of EDTA
What is the CONCENTRATION of Ca2+ ion?

What is the hardness?

Apparatus/Reagents

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50ml pipette, 250ml Erlenmeyer flask, burette, buffer, Eriochrome black T indicator,
0.001M EDTA solution, Well water, river water.
Procedure
Prepare 0.002M EDTA solution. Pipette a 50ml portion of the water samples to be analyzed into
250ml Erlenmeyer flasks. To the first sample add 1.0ml NH3-NH4Cl buffer solution and five drops
Eriochrome black T indicator. Titrate with a standard EDTA solution to a colour change of wine
red to pure blue. Repeat the procedure with the other water samples provided.

POST LAB QUESTIONS

1. Calculate the total hardness of water (in ppm) in each of the water samples.

EXPERIMENT 4
GRAVIMETRIC ANALYSIS OF SOLUBLE CHLORIDE
BACKGROUND
Gravimetric analysis is a method based on the isolation of the desired constituent in pure form or
in some combined form from a sample, and weighing the isolated constituent. The desired
constituent is usually isolated or separated by precipitation. From the weights of sample and
precipitate, the percentage constituent can be calculated.
Precipitation is affected by inorganic or organic precipitating agents. Two inorganic precipitating
agents are silver nitrate, which is used to precipitate halide ions such as chloride, and barium
chloride which is used to precipitate sulfate ion. Potassium, ammonium, rubidium and cesium ions
are precipitated by sodium tetraphenylborate. In all of these precipitation reaction, the product is
a salt because it is formed by reactions between cations and anions and the bonding is electrovalent.
Organic precipitation reagents contain functional groups which combine inorganic ions to form
insoluble salt. The organic reagent may contain groups such as carboxyl and hydroxyl which ionize
to form anions that combine with cations to form insoluble salts. In this reaction, the bonding is
also electrovalent. Some organic reagents contain nitrogen or oxygen that can combine with metal
ions by forming covalent or coordinate bonds. Other organic reagents contain two or more
functional groups which can combine with a single, can contain two or more functional groups.
The product formed between a cation and multidentate ligand, a ring is named a chelate.
Silver ions undergo the following reaction with chloride.
Ag+ + Cl+ AgCl (white solid)

Silver chloride is a relatively insoluble compound with a solubility product (Ksp = [Ag+] [Cl-]) of
1.8 10-10.

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An excess of silver ions is added so that the chloride concentration at equilibrium will be
negligible. If enough silver ions is added, the precipitation will be incomplete, resulting in a
substantial error and a low value for the % CI in the sample Reagents
• 0.01M Nitric acid
• 1M Silver nitrate

Preparation of Porcelain Crucibles

1. Clean and dry three porcelain crucibles (see notes below). Make sure crucibles are marked
so they can be distinguished from one another.
2. Dry crucibles in the oven at 100 – 110oC for one hour or overnight. The crucibles should
be put in a labeled beaker and covered with a watch glass when in the oven.
3. Cool the crucibles in a desiccator for 20 minutes and weigh.
4. Repeat this procedure until the mass of each crucible agrees to within 0.3mg

Preparation of Unknown Chloride

1. Weigh out 0.5g of NaCl into three different 500 ml beaker
2. Dissolve each portion using 100 ml distilled water

Precipitation of Chloride with Silver Nitrate

3. Heat the chloride solutions to boiling and with constant stirring add the Silver Nitrate until
the precipitation of the Silver Chloride is complete. To check for complete precipitation,
Silver Nitrate must be added in small quantities and vigorously stirred. Allow it then to
settle a bit and add some more Silver Nitrate solution (no stirring yet), if the solution
becomes cloudy, keep adding. If the solution remains clear add a little more Silver Nitrate
solution, then cool the solution in a locker

Filtration and final weighing (this procedure should be done separately for each sample)
4. After the solution has cooled, filter it through a weighed filter paper.
5. Wash the precipitate with three 25 ml portions of 0.01M Nitric acid.
6. Dry filter paper containing the precipitate in an oven at 120oC.
7. Cool the precipitate in a desiccator and reweigh

Gravimetric calculation
Calculate the % chloride in the sample.

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EXPERIMENT 5
pH AND BUFFER SOLUTIONS
We frequently encounter acids and bases in our daily life. Fruits, such as oranges, apples, etc.,
contain acids. Household ammonia, a cleaning agent, and Liquid Plumber are bases.
Acids are compounds that can donate a proton (hydrogen ion). Bases are compounds that can
accept a proton. This classification system was proposed simultaneously by Johannes Bronsted
and Thomas Lowry in 1923, and it is known as the Bronsted-Lowry theory. Thus, any proton donor
is an acid, and a proton acceptor is a base. When HCl reacts with water

HCl + H2O H3O+ + Clˉ

HCl is an acid and H2O is a base because HCl donated a proton thereby becoming Cl-, and water
accepted a proton thereby becoming H3O+.
In the reverse reaction (from right to left) the H3O+ is an acid and Cl- is a base. As the arrow
indicates, the equilibrium in this reaction lies far to the right. That is, out of every 1000 HCl
molecules dissolved in water, 990 are converted to Cl- and only 10 remain in the form of HCl at
equilibrium. But H3O+ (hydronium ion) is also an acid and can donate a proton to the base, Cl-.
Why do hydronium ions not give up protons to Cl- with equal ease and form more HCl?
This is because different acids and bases have different strengths. HCl is a strong acid than
hydronium ion, and water is a strong base than Cl-.

PRE-LAB QUESTIONS
1. Phosphoric acid, H3PO4, is a triprotic acid. Show the formula of the conjugate base after two
protons have been donated.
2. The pKa of the formic acid is 3.75. What is the pH of a buffer in which formic acid and sodium
formate have equimolar concentration? What is the pH of a solution in which the sodium
formate is 10 M and the formic acid is 1 M?
3. The pH of normal blood is 7.4. A diabetic patient‟s blood gave a pH reading of 6.4. How much
more hydronium ion (H3O+) is in the blood of the diabetic patient?

Objective(s)
• To determine how to measure pH of a solution.
• To demonstrate the operations of buffer systems.
Apparatus/Materials:
pH meter, pH paper, Kimwipes, Wash bottles, 10mL beakers

Chemicals:
0.1 M HCl,

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0.1 M acetic acid (CH3COOH),
0.1 M sodium acetate (CH3COONa),
0.1 M carbonic acid or club soda or seltzer,
0.1 M NaHCO3
0.1 M NH3 (aq) (aqueous ammonia),
0.1 M NaOH

Procedure Measurement of pH
1. Add 5mL of 0.1M HCl to a 10mL beaker. Dip a 2-cm long universal pH paper into the solution.
Remove the paper from the solution. Compare the color of the paper to the color chart
provided. Record the pH on your report sheet.
2. Repeat the same procedure with 0.1M acetic acid, 0.1M sodium acetate, 0.1M carbonic acid
(or club soda or seltzer), 0.1M sodium bicarbonate, 0.1M ammonia, and 0.1M NaOH. For
each solution, use a different cleaned dry beaker. Record your results on the Report Sheet.
3. Depending on the availability of the number of pH meters this may be a class exercise
(demonstration), or 6-8 students may use the one pH meter. Add 5mL of 0.1M acetic acid to a
dry and clean 10-mL beaker. Wash the electrode over a 200-mL beaker with distilled or
deionized water contained in a wash bottle. The 200-mL beaker serves to collect the wash
water. Gently wipe the electrode into the Kimwipes (or other soft tissues) to dryness. Insert
the dry electrode into the acetic acid solution. Your pH meter has been calibrated by your
instructor. Switch “on” the pH meter and read the pH from the position of the needle on your
scale. Alternatively, if you have digital pH meter, a number corresponding to the pH will
appear.
4. Repeat the same procedures with 0.1M sodium acetate, 0.1M carbonic acid, 0.1M bicarbonate,
and 0.1M ammonia. Make certain that for each solution you use a dry and clean beaker, and
before each measurement wash the electrode with distilled water and dry with Kimwipes.
Record your data on the Report Sheet.
5. Prepare four buffer systems in four separate, labeled, dry, and clean 50-mL beakers, as follows:
a. 5 mL 0.1M acetic acid 5 mL 0.1M sodium acetate
b. 1 mL 0.1M acetic acid 10 mL 0.1M sodium acetate
c. 5 mL 0.1M carbonic acid 5 mL 0.1M sodium bicarbonate
d. 1 mL 0.1M carbonic acid 10 mL 0.1M sodium bicarbonate
Measure the pH of each buffer system with the aid of universal pH paper. Record your data
on the Report Sheet.
6. Divide each of your buffers (a-d) into two halves (5mL each) and place them into clean and
dry 10-mL beakers. To the first sample of buffer (a), add 0.5 mL, 0.1M HCl. Mix and measure
the pH with the aid of universal pH paper. Record your data on the Report Sheet. To the second
sample of buffer (a) add 0.5 mL 0.1M NaOH. Mix and measure the pH with pH paper. Record
your data on the Report Sheet.

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Reference Materials
Peter Atkins and Julio de Paula, (2006), Physical Chemistry, Oxford University Press, United
Kingdom, 8th Edition, 1072 pp.

Harvey David. (1999), Modern Analytical Chemistry, McGraw-Hill, 1st Edition, 798 pp.

Wade L.G. Jnr. (2013), Organic Chemistry, 8th Edition, Pearson Education, ISBN 9780-321-

76841-4 (0-321-76841-8), 1326 pp.