A Compilation of Experiments and Procedures for Analytical Chemistry Lab1

A REMINDER TO THE STUDENT: GUIDELINES & POLICIES in the LABORATORY

The Lab Instructor is the first to enter and the last one to leave the Lab Room.
The students are not allowed to enter the lab room without the Lab Instructor or to stay beyond the
lab period in the absence of the Faculty in-charge.
During the First Meeting, each group is asked to check in a set of glassware and equipment for
the entire term.
The group fills up a Check in Form to confirm the contents of the cabinet assigned to them.
The members of the group are responsible for all items issued under their names and any breakage or loss
will be charged to the group.
The integrity of the items issued to the group is the sole responsibility of the group members. Be
sure that the cabinet is securely locked. Bring your own padlock and key on the Second Meeting.
The group may borrow other items from the Stock Room on an as need basis.
A member of the gro p fills p a Borro er s Slip and presents his/her ID Card. At the end of the lab
period, the gro p ret rns all borro ed items listed in the Borro er s Slip to the Lab Technician. The
st dent, in t rn, recei es his/her ID card and Borro er s Slip from the Technician.
The group will be assigned a specific work area and it is their responsibility to keep it clean and orderly.
Don t forget to ret rn all sed items (those that ere iss ed to the gro p for the entire term) inside
the locker.
Throw paper and matchsticks in the trash bin. Verify with your Lab Instructor which chemical
wastes can be flushed down the sink with running water and which ones are to be disposed in chemical
wastes containers.
Check the water faucet and gas outlet after using. Report leaks to the Lab Instructor or Technician.
Submit your updated Pre-Lab Report Notebook (also referred to as the Journal) on time.
Students will not be allowed to perform the experiment without the updated Pre-Lab Journal.
Always wear the appropriate laboratory attire. Students not wearing the appropriate lab attire will
automatically get an absence mark and will be prohibited to perform the experiment.
Sleeveless shirts, shorts, skirts and open-toed footwear are not allowed. Wear shoes that shed or repel
liquids. Always secure long hair with a clip, hair clamp or band. Remove necktie or scarf when
performing experiments.
Wear your lab gown and goggles while performing an experiment.
The lab gown and goggles are worn as long as the student is within the working area of the lab
room. Students are also required to wear the lab gown while washing/cleaning the glassware/lab items
(before and after the performance of the experiment).
NO UNAUTHORIZED EXPERIMENTATION!
Students are not allowed to perform experiments other than the one that is indicated in the procedure of
the experiment scheduled for the Day. Irresponsible mixing of solutions, esp. without proper supervision,
may result in serious accidents.
Report all accidents, no matter how minor it may appear, to the Lab Instructor.
All accidents must be recorded and students who need/require immediate medical attention must be sent
to the University Clinic.
During the Check-out Week (13th week of the Term), the students will return all the glassware and
equipment issued to the group.
The integrity of the contents of the locker is determined by comparing the contents of the locker
with the items indicated in the Check-in Form. The group will be charged for any loss or breakages and
the payment is done at the Accounting Office. The receipt is presented to the Technician in-charge and a
clearance slip will be issued to each student. The clearance must be presented to the Proctor during the
Final Exams for the Laboratory.
The Pre-Lab Journal, the Compilation of the Exercises/Assignments, ASA, Data and Calculations Sheet
and Final Report Sheet are submitted to the Lab Instructor during the Final Exam Week.

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LABNotes: Tools of Analytical Chemistry

The demands on the analytical chemists have increased over the recent years. It is expected that the
results must have a high level of confidence, high precision, update on the recent developments in the
analytical techniques, instrumentation and automation and an increase in the number of samples to be
analyzed.

The analyst always refers to the OFFICIAL METHODS OF ANALYSIS as a major reference for
procedures to be used in every analytical work. The ASSOCIATION OF OFFICIAL ANALYTICAL
CHEMISTS major contribution to analytical science has been to bring the collaborative study technique
for the validation of analytical methods to a high degree of perfection.

It aims to establish the performance characteristics of the process in terms of accuracy, precision,
sensitivity, range, specificity, limit of detection, limit of reliable measurement, selectivity and practicality.
The analysis of very carefully prepared samples aims to establish not only the performance
characteristics of the method but of the analyst or the lab as well.

FOR ANALYTICAL WORK, it is important that the analyst must be able to develop and refine the basic
skills and lab techniques learned from general chemistry labs.

1. Selecting and Handling Reagents and Other Chemicals:

Proper Choice of Reagents

Chemicals are classified based on the purity or the results of the assay as reported by the manufacturer
Reagent Grade Chemicals (AR Grade)
Conform to the minimum standards or specifications set by the Reagent Chemical Committee of
the American Chemical Society (ACS)
Used for analytical work
Container Label contains information regarding the maximum limits of impurity

Primary Standard Grade

99.99% purity and specifications of the maximum limits of the impurities present. Not all
substances can exists as primary standard grade
The results of the assay are printed on the container label

Special Purpose Reagent Chemicals

Used for a specific application like:
HPLC Grade solvents are used for HPLC
Spectrophotometric Grade Solvents contain information regarding its absorbance at
selected wavelengths and its UV cut-off wavelength

Other Grades (Not Suitable for Analytical Work)

Technical Grade only for cleaning purposes
Chemically Pure no assay provided
USP Grade suitable for pharmaceutical purposes only

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2. Measurement – assignment of numbers to objects, events, properties

4 kinds of Scales namely

a. nominal scale assign a single number to each object
b. ordinal scale arrange objects/events in rank or order and requires an additional
numeral operation determining greater or less
c. interval scale determination of the equality of intervals or differences; such is the
measurement involved in quantitative measurements
d. ratio numerical operations for determining 2 relations: equality, rank order, equality of
interval and equality of ratios

Physical and chemical measurements involve the last 2 scales.

a. Measurement of Mass
Types of Balances
An analytical balance is an instrument used for determining the mass with a maximum
capacity that ranges from 1 g to a few kg and a precision at maximum capacity of at
least 1 part in 105 to 1 part in 106

Analytical balance is used for highly accurate measurements; 1 part in 105 of its
maximum capacity or even 1 part 106 of its full capacity.

Tare is the mass of an empty sample container.

Taring is the process of setting a balance to read zero in the presence of the tare.
Taring control causes the display to read zero with a container on the pan.

A laboratory balance or auxiliary balance is rugged and with less sensitivity than an
analytical balance. Ex. platform balance

Sources of Error in Weighing

Buoyancy Error is the weighing error that develops when the object being weighed has a
significant difference in density with the standard masses.

Temperature Effects
Convection currents within the balance case exert a buoyant effect on the pan and object
Warm air trapped in a closed container weighs less than the same volume at a lower
temperature

Both effects cause the apparent mass of the object to be low and can amount to as much as 10
to 15 mg.
Heated objects must always be cooled to RT before weighing

Other Sources of Error

Static charge serious when the relative humidity is low
Check the optical scale regularly for accuracy

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Drying or Ignition to Constant Mass a process in which a solid is subjected to several cycles of
heating, cooling and weighing steps until its mass becomes constant to within 0.2 to 0.5 mg.
Hot objects look the same at cold ones.

Weighing Bottles are used for drying, storing and weighing solids

A dessicator is a device for drying substances or objects.

Used to store heated objects or substances to minimize the uptake of moisture while they
cool to RT
It contains a chemical drying agent called a dessicant.
Examples of drying agents are anhydrous CaCl2, CaSO4 (Drierite), Mg(ClO4)2 (Anhydrone or
Dehydrite)
The ground glass surface are lightly coated with grease
The lid or cover of the dessicator is removed with the use of a sliding motion

Methods Used in Weighing

Weighing by Difference.
The weighing bottle with the sample is weighed initially. The desired quantity of the
sample is obtained and transferred into a clean, dry container. The weighing bottle
and the remaining contents are weighed again. The decrease in the mass of the two
measurements represents the mass of the obtained sample.
Weighing by Addition
The mass of the empty weighing bottle is measured. The desired quantity of the
sample is added to the weighing bottle. The weighing bottle and the sample are
weighed together. The increase in the mass of the two measurements represents the
mass of the obtained sample.

b. Measurement of Volume
SI unit for volume is cubic decimeter or dm3.
1 liter (L) = 1 dm3 1000 mL = 1 L
1 mL = 1 x 10-3 L 1 L = 1 x 10-6 L = 1 x 10-3 mL

Apparatus Used for Precise Measurements of Volumes of Liquids

Glassware Designed To Deliver (TD) Liquids

a. Measuring Pipet
b. Volumetric or Transfer Pipet
c. Buret

Glassware Designed To Contain (TC) Liquids

Volumetric Flask

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An experiment is an investigation of the relationship between a dependent and independent variable.

In general, only 1 variable to change and the rest are held constant. The following are ways by which
the change in variables are observed:

Maximum and minimum values or range

Number of values
Relationship between the dependent and independent variables
How much error can be tolerated

Characteristics of an Experiment
1. Must have a clear and cognitive purpose
2. It is selective wherein a portion of the Universe is selected for study (system). The variables of
the system must be defined.
3. It must have a beginning, middle and an end. And the change in the system is deliberately
provoked or carried out.
4. The change must be capable of being
(b) observed using either direct perception (or direct method) using the eyes or indirect
measurement involves the use of an instrument
(c) interpreted by the observer and recognize the change as a significant difference in a
variable property of the system
(d) described by observer and recorded in such as way that it can be communicated to
another scientist for testing or reproduction
5. The system and the change should be reproducible and testable by other scientists

Collection of Data
Best done in a sequential manner that is from lowest to highest or vice versa
Establish the relationship between the dependent and independent variables
If the relationship is linear then collect data such that there is equal spacing between
values
If the relationship exhibits an inflection point then y is slowly changing with x. the x
values may be more widely spaced However near the inflection point the x values must
be chose close together so that the changes in y are kept more or less constant between
all changes
If the data shows a maximum then the data can be more widely spread near the base of
the peak where y is changing very slowly with x. Then it is more closely spaced on the
sides where y is changing rapidly. This allows the location of the maximum more
precisely.
Keeping records.
Resist temptation to perceive observations to support the hypothesis or distort unsupportive
observation to minimize disagreement. Exercise absolute objectivity and avoid prejudice,
bias and fraud.
Bias interferes with the testing of the hypothesis.

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A chemist seeks a relationship between a property and what is observed. It is necessary to report not
only the quantitative relationship and the value of a calculated property but also some measure of the
reliability of the measurements and subsequent calculations.

Therefore one must report the calculated value and the error d .

Measurements are repeated in order to test the reproducibility of the experiment and gain confidence in
the accuracy of the results.

TYPES OF ERRORS IN EXPERIMENTAL DATA are random and systematic errors

1. RANDOM or INDETERMINATE ERROR
Causes data to be scattered more or less symmetrically around a mean value.
It occurs with a different sign and magnitude each time an experiment is executed.
Positive and negative errors are equally likely to occur
It affects measurement precision. All measurements contain random errors and can never
be totally eliminated. It is often the major source of uncertainty in a determination.
Even when prejudice is eliminated, random human errors arise from unpredictable
psychological and physiological limitations inherent in human experimentation.
An experiment with small random errors is precise.
Caused by the many uncontrollable variables that are an inevitable part of every analysis. It
is caused by unpredictable mechanical and electrical fluctuations affecting the operation of
instruments and experimental apparatus.

The spread or the range is used to describe the precision of a set of replicate measurements is the
difference between the highest and the lowest result. It results directly from an accumulation of all
random uncertainties in the experiment.

Example: Sources of random uncertainties in the calibration of a pipet include

(1) visual judgments of the level of the water with respect to the marking on the pipet or the Hg
level in the thermometer
(2) variations in the drainage time and the angle of the pipet as it drains
(3) temperature fluctuations which affect the volume of the pipet, viscosity of the liquid and the
performance of the balance
(4) vibrations and drafts that cause small variations in the balance readings

The cumulative influence of these variables is responsible for the observed scatter of results around
the mean.

2. SYSTEMATIC or DETERMINATE ERROR

Affects the accuracy of the results. An experiment with small systematic errors it is accurate.
Causes the mean of a data set to differ from the accepted value
It causes all the results in a series of replicate measurements to be too high or too low. For
example, a loss of a volatile analyte while the sample is being heated.
Systematic errors have a definite value and an assignable cause, and are of the same magnitude
for replicate measurements made in the same way.
Leads to bias in measurement results. Bias measures the systematic error associated with an
analysis. It has a negative sign it causes the results to be low and a positive sign if it causes the
results to be high.
It can be AVOIDED!

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3. GROSS ERROR
Occurs occasionally, often large and may cause a result to be either high or low.
It is often a product of human errors
For example, loss of precipitate during weighing will cause the results to decrease.
It leads to outliers. An outlier is an occasional result in replicate measurements that differs
significantly from the rest of the results.

There are 3 types of systematic errors:

(1) INSTRUMENTAL ERRORS are caused by nonideal instrument behavior by faulty
calibrations or use under inappropriate conditions.
All measuring devices are potential sources of systematic errors.
Calibration eliminates most systematic errors of this type.
Pipets, burets and volumetric flasks must be calibrated because they may hold or deliver
volumes slightly different from those indicated by their graduations due to temperature
fluctuations.
Electronic instruments are subject to instrumental systematic errors. This is largely due
to power supply fluctuations. Similar errors are detectable and correctable.

EXAMPLES OF INSTRUMENTAL AND REAGENT ERRORS

Faulty construction of balances
Improperly calibrated weights, graduated glassware and other instruments
Attack of reagents upon glassware, porcelain, etc.
Introduction of foreign materials
Use of reagents containing impurities

(2) METHOD ERRORS are difficult to identify and correct.

The systematic method errors are the most serious type of systematic error. It includes
slowness of some reactions, incompleteness of reactions, instability of some chemical
species, indicator error, incomplete combustion of the sample.

EXAMPLES OF ERRORS OF METHOD

Most serious because it is difficult to detect
Examples: the pH meter is wrongly calibrated; background absorption in AAS; faulty detector
response in chromatographic and spectroscopic methods
Errors in classical analysis
Examples: solubility of the precipitate; decomposition or volatilization or ignition of weighed
substance in gravimetric analysis; choice of observed end point and equivalence point
Matrix effects is the difference in bulk composition of analyte sample solution and the
composition of the standard solutions

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(3) PERSONAL ERRORS

Most measurements require personal judgments like estimating the position of a pointer
between two divisions, the color at the endpoint or the level of the liquid with respect to
graduations in a pipet, buret or graduated cylinder.
Judgments of this type are often subject to systematic, unidirectional errors. An analyst
may be insensitive to color changes, may read a pointer consistently high or tend to use
an excess reagent in a volumetric analysis.
The universal source of personal error is prejudice or bias.

EXAMPLES OF OPERATIONAL AND PERSONAL ERRORS

Due to factors for which the individual analysts is responsible and are not connected with the
method or proced re personal eq ation
Mostly physical in nature
Occurs when an analyst does not follow sound ANALYTICAL TECHNIQUES
(a) incomplete drying of samples before weighing
(b) mechanical loss of materials during sample dissolution exp. When accompanied by
effervescence or bumping
(c) incorrect technique involving the transfer of solutions
(d) lack of reproducibility in solvent extraction methods

errors during sample treatment is the major source of error in chemical analysis.
Personal errors due to judgment of color changes during visual titration causes overstepping of
end point
Estimation of values between scale divisions

EFFECT OF SYSTEMATIC ERRORS ON ANALYTICAL RESULTS

a. Constant Errors
Independent of the sample size being analyzed
Stay essentially the same as the size of the quantity measure is varied. The absolute error
remains constant with sample size but the relative error changes with changes sample size.
It becomes more serious as the size of the sample decreases.

b. Proportional Errors
Increase or decrease according to the size of the sample taken for analysis. The absolute
error varies with sample size but the relative error stays constant with changing sample size.
Due to the presence of interfering contaminants in the sample
Systematic instrument errors can be found and corrected by calibration. Periodic calibration of the
equipment is desirable because the response of the instrument changes with time, overuse, etc.

Most personal errors can be minimized by training, self-discipline and care.

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Errors in Chemical Analysis

Error is the difference between a measured value and the true value (the known or accepted value). It
is also the estimated uncertainty in a measurement or experiment

Errors are caused by faulty calibration or standardization, random variations and uncertainties in results

Measurements are always influenced by uncertainties and these cause the results to scatter.

Accuracy is the closeness of a meas rement to the tr e or accepted tr e al e

Absolute error, E = xi where is the true value

Relative error (%), ER =

xi
100

Precision is the closeness of results among one another obtained in exactly the same way;
reproducibility of measurements

Deviation, d = xi - x
2
xi x
Standard deviation, s =
n 1

s
% Coefficient of Variation, CV = 100 (Note: The CV is also referred to as %RSD)
x
s
% Relative Standard Deviation, RSD =
100
x

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Experiment 1
Analysis of Impure Sodium Carbonate

Introduction:
Chemicals and reagents are graded and classified based on the relative amounts of the analyte and
the impurities present in the sample. The composition of the representative sample of the reagent is
expressed in terms of its % analyte present. Old and unlabelled reagent bottles must be analyzed prior to
use in order to determine its purity.
The sample to be analyzed contains Na2CO3 and an inert impurity. For this kind of sample, the
direct titration of the sample with a standard solution of hydrochloric acid until the methyl orange end
point is sufficient. At the methyl orange end point, the titration reaction is shown below:
Na2CO3 + 2HCl 2NaCl + 2 H2O + CO2

Experimental Procedure
1. Preparation of 0.1M HCl
Pipet 8.5 ml of concentrated HCl to a clean glass-stoppered bottle containing approximately
900 mL of distilled water. Stopper the bottle and mix the solution thoroughly. Label the bottle.

2. Standardization of 0.1M HCl against the Primary Standard Sodium Carbonate, Na2CO3
Label three dry and clean 250-mL Erlenmeyer flasks as trial 1, trial 2 and trial 3. A reagent
bottle that contains a previously dried primary standard grade Na2CO3 (M. M. = 105.99 g/mole)
will be provided for the class. From this reagent bottle, obtain approximately 1 g of the Na2CO3 and
transfer it into a clean and dry 50-mL beaker.
Triplicate samples of accurately weighed primary standard grade or pure Na2CO3 must be
obtained for the standardization of the HCl solution. Read and understand the procedure described
below.
With the use of an analytical balance, accurately weigh the beaker containing the pure Na2CO3.
Record the value on the laboratory notebook under the heading trial 1 across the description, mass
of beaker plus Na2CO3. Obtain a portion of the Na2CO3 and transfer it into the first Erlenmeyer
flask. Reweigh the beaker and the remaining contents. Record the value under the heading mass
of beaker less Na2CO3. The difference must lie within the range of 0.10 and 0.15 g.
Repeat the same procedure until all three flasks contain pure sodium carbonate, Na2CO3.
Calculate the mass (g) Na2CO3 obtained for each trial.
Dissolve the Na2CO3 in about 40-60-ml distilled water and add 2 to 3 drops of methyl orange
indicator solution. With a white board under the flask, the solution must appear yellow in color.
Rinse the buret with about 20 mL of the prepared HCl solution and discard the rinsing down the
sink. Pour HCl solution into the buret and fill in the air gap. You may need to pour more HCl into
the buret. Wipe the buret to remove any excess acid solution.
Record the initial buret reading and titrate the solution containing the sodium carbonate with the
HCl solution until the methyl orange end point. This is indicated by the appearance of a permanent
faint pinkish orange cololr that will persist for about 30 seconds.
Note: Prepare 1.0 g KHP in 100.0 mL distilled water and add 2 to 3 drops of the methyl orange
indicator solution. This is the color that must be observed at the end point of the titration.

Repeat the titration with the other two samples, recording all data in the Lab Journal.

Report the molar concentration of the HCl standard solution.

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3. Determination of Na2CO3 in an Impure Sample

Each group will be given an unknown based on your Group Number. The group will receive 3
packets containing the unknown sample. The samples were prepared such that their composition are
the same.
Obtain one of the three (3) packets and weigh using an analytical balance. Record the mass of
the first packet. Transfer the contents of the packet into a dry Erlenmeyer flask and label the flask
as trial 1. Weigh the empty packet and record its mass. The mass of the sample can be
determined from the difference between the two mass readings. Do the same for the other two
packets of samples. Always remember to label the Erlenmeyer flask according to the sample it
contains.
Dissolve the unknown in about 40-60 ml of distilled water and add 2 to 3 drops of methyl
orange. Titrate with the hydrochloric acid solution with constant swirling until the appearance of a
pinkish-orange color for about 30 sec. Repeat the same procedure with the other 2 samples.

Report the composition of your sample in terms of %(w/w) Na2CO3.

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Experiment 2
Determination of Acetic Acid in Vinegar See Canvas for Online Simulation Procedure

Introduction
The total acid content of a sample of vinegar is readily determined by the direct titration with a
standard solution of a strong base. The acidity of vinegar is usually expressed in terms of the percentage
of acetic acid, CH3COOH, present in the sample. The analyte, acetic acid, is a monoprotic weak acid.
Although the chemical formula, CH3COOH, indicates that there are four (4) hydrogen atoms, only one is
considered acidic or ionizable. The acidic H is the one contained in the carboxylic acid group, COOH.
This hydrogen is referred to as the titratable H because it is the one that will react with the titrant
solution, NaOH.
The composition of most liquid commercial products is expressed in terms of mass to volume
percent. This concentration unit is differentiated from the mass percent by writing the symbol (w/v) or
(wt/vol) after the value of the composition. Commercially available vinegar products have a
concentration of 4% to 6% (w/v) CH3COOH. This means that the vinegar contains 4-6 g acetic acid per
100 mL of the vinegar sample.
The vinegar sample will be analyzed using titration of aliquot portions. An aliquot is a portion
taken from the sample that is a representative of the bulk. The aliquot is assumed to have the same
composition as the bulk and is homogeneous. This means that the concentration of the aliquot is the
same as the concentration of the solution from which the aliquot was obtained.
An aliquot portion of the vinegar (not the entire vinegar present in the bottle) will be obtained and
diluted to an accurate volume with the use of the volumetric flask. From this dilute vinegar solution,
triplicate portions of equal volumes (aliquots) will be measured and titrated with the standard solution of
the strong base. Observe that what is being titrated is just a fraction (portion) of the entire bottle.
However, after incorporating the dilution factor, the concentration of the aliquot portion will be the same
as what will be obtained if the entire vinegar in the bottle was titrated.

Experimental Procedure
1. Preparation of 0.1 M NaOH
Boil approximately 1L of distilled H2O. Be sure to protect the water from the atmosphere as it
cools. Measure 4 to 5 mL of a previously prepared 50% NaOH and add it to the distilled H2O.
Securely cover the bottle with a polyethylene cap and mix the solution thoroughly. Label the bottle.
Protect the solution from unnecessary exposure to the atmosphere.

2. Standardization of 0.1M NaOH Against Potassium Hydrogen Phthalate

Obtain three dry and clean 250-mL Erlenmeyer flasks and label each one. Accurately weigh
(ranging from 0.3 and 0.7 g) triplicate samples of pure, previously dried potassium hydrogen
phthalate (KHP) and carefully transfer into each flask. Record the mass (g) of the KHP present
in each flask. Dissolve each sample in about 50-70 ml distilled water and add 2 to 3 drops of
phenolphthalein solution to each flask. Set aside.
Pour about 100 mL of the 0.1 M NaOH solution into a 250-mL beaker and label the container.
Cover the beaker with a watch glass to prevent contamination.

Important! The physical appearance of the dilute NaOH solution is identical with
distilled water. LABEL the beaker with 0.1 M NaOH.

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Fill the buret with the prepared NaOH solution. Record the initial buret reading and titrate the
solution containing the dissolved potassium hydrogen phthalate with the NaOH solution until the
phenolphthalein end point. This is indicated by the appearance of a permanent faint pink color
that will persist for about 30 seconds. Recorde the Repeat the titration with the other two
samples, recording all data in the Lab Journal.

Report the molar concentration of the NaOH standard solution.

3. Determination of Acetic Acid In Vinegar

A. Preparation of the Dilute Sample Solution (DSS)
With the use of a volumetric pipet, draw 25.00-ml of vinegar into a 250-ml volumetric flask, dilute
to the mark, and mix thoroughly. Label the solution as dilute sample solution (DSS).

B. Titrimetric Analysis of the Dilute Sample Solution (DSS)

With the use of a volumetric pipet, transfer 25-mL of the dilute sample solution into an
Erlenmeyer flask and add 2 to 3 drops of the phenolphthalein indicator. Titrate with the
standard NaOH solution to the first permanent pink color. Repeat the titration with two more 50-
mL aliquot portions of the dilute vinegar.

Report the results of the analysis in terms of % (w/v) CH3COOH in the vinegar sample

Notes:
1. Do not handle NaOH pellets with fingers. This substance is corrosive.
2. Never use a glass-stoppered bottle to store the prepared NaOH solution. The NaOH will
cause the glass to freeze making it difficult, or sometimes impossible to open the bottle. It is
for the same reason that one should not use a buret with a glass-stopcock for titration
involving NaOH solution.
3. Store the remaining standard NaOH solution for succeeding experiments.
4. Dry KHP in the oven at 105 110oC for two hours or more.
5. The mass (g) of the weighed primary standard must lie within the same value until the first 2
significant figures.
6. To avoid spattering, be sure to have the tip of the buret near the surface of the solution being
titrated then add NaOH solution. Avoid splashing drops upon the sides of the flask.
7. Always use a volumetric or transfer pipet when measuring aliquot portions.

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Experiment 3-4
Potentiometric Titration of Acids and Bases
Graphic Determination of End Point See Canvas for Dry Lab Procedure

Introduction:
When choosing the best visual indicator to use for a titrimetric analysis, one must be
knowledgeable of the changes in the properties of the titration mixture as the reaction progresses. In an
acid-base reaction, this is determined by monitoring the change in the pH of the reaction mixture as the
titrant is added. The visual indicator is chosen so that the change in color of the indicator occurs at the
stage very close to the equivalence point of the reaction. In the absence of a satisfactory visual
indicator, graphical determination of the end point is the best way to determine the equivalence point.

During the titration of the acid or base, the potential between two electrodes dipped in the analyte
solution is monitored as the titrant is added. One of the electrodes is an indicating electrode, which is a
glass electrode, normally the standard calomel electrode (SCE), with an invariant potential. Nowadays,
combination electrodes are widely used, where both indicating and reference electrodes are combined in
one compartment.
The equivalence point in the titration is determined by plotting, pH vs the volume of titrant added.
A sharp break in the titration curve is observed in the vicinity of the equivalence point. The equivalence
point in the titration curve can be determined by extending 2 straight lines (A and B) along the lower
and upper curve that comes before and after the sharp rise or inflection curve. Two parallel lines are
drawn along y-axis before and after the inflection curve. A third line is drawn through the midpoint of
the two parallel lines. The equivalence point is the point where the middle line intersects the titration
curve. The corresponding volume is the equivalence point volume.

Titration Curve: Strong Acid-Strong Base

Reaction

14.000
12.000
10.000
8.000
pH

6.000
4.000
2.000
0.000
1.00
6.00
11.00
16.00
21.00
26.00
31.00
36.00
41.00
46.00
51.00
56.00
61.00
66.00
71.00

Volume (mL) Titrant

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 A Compilation of Experiments and Procedures for Analytical Chemistry Lab1
Experiment # 3 Part A
Titration Curve: Strong Acid-Strong Base Reaction See Canvas for Dry Lab Procedure

Experimental Procedure:
1. Use of the pH meter.
(a) Wash the electrode with distilled water each time it is to be used.
(b) Squirt the electrode with distilled water with the use of a wash bottle. Always wipe the
electrode with tissue paper using light strokes.
(c) Before using, calibrate the pH meter in a buffer solution of pH 7 for upper calibration or pH 4
for lower calibration.

2. Preparation of Standardized 0.1M NaOH

Use the standardized 0.1M NaOH used in the previous experiments.

3. Analysis of Unknown Solution of a Strong Acid

A. Preparation of the Dilute Unknown Solution
Measure 25-mL of the unknown strong acid sample and transfer into a 250-mL volumetric
flask. Dilute the unknown acid to the mark with distilled H2O. Mix the solution thoroughly.
Label the solution as dilute acid unknown solution.

B. Titration of the Dilute Unknown Solution: Visual Indicator End Point

Pipet a 25-mL aliquot portion from the dilute strong acid unknown solution and add 2-3
drops of phenolphthalein. Titrate the dilute acid unknown solution with the 0.1 M sodium
hydroxide solution until the phenolphthalein end point. Measure the pH at the end point.
Perform a total of 3 trials.

Report the molarity of the unknown solution of the strong acid.

C. Titration Curve of a Strong Acid-Strong Base Reaction: Graphical Determination of the

Equivalence Point
a. Pipet a 25 ml aliquot portion from the dilute acid unknown and transfer this into a 100ml
beaker. Measure the initial pH reading of the solution. Add 2-3 drops of phenolphthalein
indicator solution and measure the pH reading.
b. Add 0.50 ml increment volumes of the standard NaOH solution. Stir the solution after each
addition and allow enough time to obtain a constant reading. Record the pH reading.
c. As additional volumes of the base are added, observe any changes in the color of the
solution that may happen.
d. Repeat step b until a large increase in pH reading is observed. At this point, add 6 more 1.0
ml portions of the titrant, recording the pH after each 1.0 mL addition.
e. Rinse the electrode with distilled water after using.

Prepare a potentiometric titration curve by plotting pH against volume of base titrant. Identify the
end point of the titration and the volume (mL) of the titrant needed to reach the end point. Shade the
area where the phenolphthalein end point occurred.

Report the molar concentration of the unknown solution of the strong acid for each trial and make a
comparison of the concentration for the 2 methods.

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 A Compilation of Experiments and Procedures for Analytical Chemistry Lab1
Experiment # 3 4 Part B
Titration Curve: Weak Acid-Strong Base Reaction See Canvas for Dry Lab Procedure

Experimental Procedure:
4. Determination of the Acid Dissociation Constant, Ka of a Weak Acid
Note: Each group will be assigned a specific weak acid as unknown.

A. Preparation of the Dilute Acid Unknown

Measure a 25-mL aliquot of the unknown acid solution and transfer into a 250-mL
volumetric flask. Dilute the unknown acid to the mark with distilled H2O. Mix the solution
thoroughly. Label the solution as dilute acid unknown.

B. Titration of the Dilute Acid Unknown Using Phenolphthalein as the Visual Indicator
a. Pipet a 25 ml aliquot portion from the dilute acid unknown and transfer this into a 100ml
beaker. Measure the initial pH reading of the solution. Add 2-3 drops of phenolphthalein
indicator solution and measure the pH reading. Do you observe a change in the pH
reading?
b. Titrate the solution until the phenolphthalein end point. Record the buret reading.
Measure the pH of the resulting mixture. Repeat the titration for a total of 3 trials using
25-mL aliquot portions. Results must agree to at least 0.1 mL. Calculate the average
volume of NaOH needed to reach the phenolphthalein end point.
c. Pipet a fourth 25-mL aliquot portion from the dilute acid unknown. Measure the initial pH
reading.
d. Titrate the solution until only one-half of the average volume of the NaOH solution
needed to reach the phenolphthalein end point has been added. Measure the pH of the
mixture.
e. Repeat procedures c and d for two more additional trials.

C. Potentiometric Titration of the Dilute Acid Unknown

a. Obtain a 25-mL aliquot of the dilute acid unknown and transfer it into a 50 or 100-mL
beaker. Measure the initial pH of the solution.
b. Add 0.5 ml increment volumes of the standard NaOH solution. Stir the solution after
each addition and allow enough time to obtain a constant reading. Record the pH
reading.
c. Repeat step b until a large increase in pH reading is observed. At this point, add 6 more
1.0-ml portions of the titrant, recording the pH after each 1.0 mL addition.
d. Rinse the electrode with distilled water after using.

Prepare a potentiometric titration curve by plotting pH against volume of base titrant. Identify the
end point of the titration and the volume (mL) of the titrant needed to reach the end point. Shade the
area where the phenolphthalein end point occurred.

Compare the pKa obtained from the two methods. Check your experimental values with the value
obtained from the Table of the Acid Dissociation Constant.

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 A Compilation of Experiments and Procedures for Analytical Chemistry Lab1
Exercise 4 6
Experiment
Determination of Hydrogen Peroxide in Antiseptic Solutions

Introduction:
Potassium permanganate has a very high oxidizing power with a reduction potential of 1.507 V.

MnO4- + 8 H+ + 5 e- Mn2+ +4 H2O

In titrimetric analysis, it is frequently used as titrant due to its intense coloring power, which requires no
auxiliary indicator. When the titration is carried out in acidic medium, the permanganate ion is reduced
to the colorless manganous ion (Mn2+) in aqueous solution. A drop of excess permanganate turns the
solution into pink color, which could last for about 15 seconds. This color is taken as the endpoint of the
titration. The solution readily decomposes to brown MnO2 upon reaction with heat, sunlight or organic
contaminant.

Experimental Procedure
1. Preparation of a 0.02 M Potassium Permanganate.
Weigh approximately 0.8-g of a good grade potassium permanganate and place it in a 250-ml
beaker. Dissolve the salt by adding 50-ml of water and stirring. Decant the solution into a large
beaker and add 50-ml of additional water to dissolve the crystals remaining in the first beaker.
Repeat this procedure until all crystals are dissolved. Dilute the solution until the total volume of
distilled water added is about 250 mL. Transfer the solution to a glass stoppered bottle and label
properly.

2. Standardization of Potassium Permanganate Solution (McBride Method)

Accurately weigh three samples of about 0.20 to 0.25 g each of dried sodium oxalate into clean
250-ml Erlenmeyer flask. Dissolve each sample in about 75-ml of 0.75 M Sulfuric acid (20-ml of
concentrated H2SO4 added to 400ml water). Then heat the first solution to almost boiling point (80
to 90oC) and titrate slowly with the permanganate through constant swirling. The endpoint is
marked by the appearance of a faint pink color that persist for 30 seconds. The temperature should
not drop below 60oC during titration. Titrate the two other solutions in the same manner.
Add permanganate solution dropwise to about 75-ml of 0.75 M H2SO4 until the color matches
that of the titrated solution. This volume should be subtracted from the volume used in the titration.
Report the molarity of the permanganate solution.

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 A Compilation of Experiments and Procedures for Analytical Chemistry Lab1

3. Determination of Hydrogen Peroxide:

Commercial samples of hydrogen peroxide are encountered as aqueous solutions of containing about
6%-30% (w/v) H2O2. A more common way of expressing the composition of these commercial
products is by indicating the volume of oxygen liberated when the solution undergoes decomposition
by boiling. The decomposition reaction is represented by the chemical equation below:

2H2O2(aq) 2H2O(l) + O2(g)

Thus 1 mL of a sample of hydrogen peroxide with the label 100-volumes will yield 100 mL of O2
measured at standard temperature and pressure (STP). The label 20-volumes refers to a 6% (w/v)
H2O2, 40-volumes is also 12% (w/v) H2O2, and 100-volumes hydrogen peroxide refers to 30% (w/v)
H2O2.

For this experiment a 10-volume or 20-volume solution is an appropriate sample to use.

Transfer a 25 mL aliquot of a 20-volume solution to a 500 mL volumetric flask and dilute to the
mark. Label this as dilute sample solution. Measure a 25 mL aliquot portion of the dilute sample
solution and transfer into an Erlenmeyer flask. Add 20 mL of distilled water, 20 mL of dilute H2SO4
solution (1:5 dilution) and titrate with 0.02 M KMnO4 to the first permanent faint pink color. Repeat
the titration to two consecutive determinations and the trials should agree within 0.1 mL.

Express the concentration of the sample in terms of %(w/v) H2O2.

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 A Compilation of Experiments and Procedures for Analytical Chemistry Lab1
7
Experiment 4
Iodometric Titration: Analysis of a Household Bleaching Agent

Introduction:
Due to the relatively weak strength of I2 as an oxidizing agent, there are limited substances that
can be titrated with it. Other titration methods that involve the substance I2 is the indirect titration of I2
with sodium thiosulfate, Na2S2O3, and back-titration of I2 with sodium thiosulfate. In the indirect
titration of I2, the preliminary step involves the formation of I2 from the reaction of the oxidizing agent
with KI. The liberated I2 is then titrated with the sodium thiosulfate solution.

Experimental Procedure:
1. Preparation of 0.1 M Sodium Thiosulfate
Boil 500 mL of distilled water for 2 minutes and let cool. Weigh out 12.50 g Na2S2O3 5H2O
and dissolve the crystals in the previously boiled distilled H2O. Add 0.1 g Na2CO3 as a preservative.

2. Standardization of 0.1 M Na2S2O3

Prepare a 100 mL standard solution of 0.01M KIO3 from a primary standard grade KIO3.
Measure 25 mL pipetful of 0.01 M KIO3 solution and transfer into an Erlenmeyer flask. Do not add
the solid KI until you are ready to titrate. Add 25 mL of distilled H2O and 2 g of solid KI. Swirl the
contents of the flask slowly and 10 mL of 1 M H2SO4. Mix the mixture until all solids dissolve. The
release of I2 is indicated by the appearance of a deep brown color. Titrate immediately with the 0.1
M Na2S2O3 solution until the brown color fades to a pale yellow. Then add 5 mL starch indicator
and continue the titration until the blue color disappears. Record the volume of titrant delivered.
Perform the procedure in 3 trials.

Report the molarity of the sodium thiosulfate.

3. Measuring the Density of the Household Bleach

NOTE: To avoid the irritating odor of the bleach, wear a filter mask when doing the experiment.
Record the mass of a clean, dry beaker. Add 10-mL pipetful of the household bleach into the
beaker and measure the total mass of the beaker and household bleach. Record the total mass of
the beaker and the household bleach. Discard the household bleach into the sink and flush with a
lot of tap water.

4. Analysis of a Household Bleaching Agent

A. Preparation of the Dilute Bleach Solution for Analysis
Pipet 25 mL of the bleaching agent into a 250-mL volumetric flask and add enough
distilled H2O until the solution reaches the etched mark. Mix the solution thoroughly. Label the
solution.
B. Titration of the Dilute Bleach Solution
Pour 50 mL of distilled H2O in a 250 mL Erlenmeyer flask and dissolve 2 g of solid KI.
Add a 25-mL pipetful of the dilute bleaching solution to the flask and swirl the mixture until all
solids are dissolved. Slowly add 25 mL of 1M H2SO4, 5 drops of 3% ammonium molybdate
catalyst and mix. Allow the mixture to stand for about 1 to 2 min. Titrate the mixture with 0.1 M
Na2S2O3 solution until the mixture turns to pale yellow. Add the 5 mL starch indicator and
continue titrating until the blue color disappears. Perform the analysis in 3 trials.
Note: Adjust the volume of the dilute bleaching solution to be titrated if the volume of the titrant
needed to reach the end point is less than 10 mL or more than 1 buretful.

Report the %(w/w) NaOCl.

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Experiment 5 – Online Lab
Determination of Concentration of KMnO4 Solution (http://amrita.olabs.edu.in/?sub=73&brch=8&sim=115&cnt=1)
 A Compilation of Experiments and Procedures for Analytical Chemistry Lab1
Experiment 68
Iodimetric Titration of Vitamin C See Canvas for Online Simulation Procedure

Introduction:
The ability of I2 as an oxidizing agent, there are limited substances that can be titrated with it.
Another titration method involving the substance I2 is the indirect titration of I2 with sodium thiosulfate,
Na2S2O3. of the back-titration of I2. In the indirect titration of I2,, preliminary step involves the
formation of I2 from the reaction of the oxidizing agent with KI. The liberated I2 is then titrated with the
sodium thiosulfate.

Experimental Procedure:
1. Preparation of 0.025 M I2
Transfer 10 mL of 0.5 M I2 solution into an amber bottle (1-L capacity) and add 200 mL of
distilled H2O. Cover the bottle and mix the solution thoroughly.

2. Standardization of 0.025 M I2
a. Preparation of Ascorbic Acid Standard Solution
Weigh accurately 0.25 to 0.45 g pure ascorbic acid and dissolve in 50 mL of distilled H2O.
Transfer into a 250-mL volumetric flask and dilute to the mark. Cover the flask and mix
thoroughly.
Report the concentration of the ascorbic acid solution in molarity.

b. Titration of Ascorbic Acid with I2

Pipet a 50-mL aliquot portion of the ascorbic acid standard solution and add 1 mL of starch
solution. Stir thoroughly and titrate with the I2 solution (prepared in number 1) until the
appearance of a distinct blue color. Repeat the procedure with two other aliquot portions of the
ascorbic acid standard solution.
Report the molar concentration of the I2 solution

3. Analysis of Vitamin C Samples

a. Preparation of Dilute Vitamin C Sample Solution
Choose an over the counter (OTC) Vitamin C (250 mg) tablet. Weigh out 2 tablets of the
vitamin sample and transfer into a 100-mL beaker. Dissolve the tablet in 100 mL of distilled
H2O. Filter the mixture and collect the filtrate into a 250-mL volumetric flask. Wash the residue
with three 20 mL portions of distilled water and combine the washings with the filtrate in the
volumetric flask. Dilute to the mark and mix thoroughtly.

b. Titration of the Dilute Vitamin C Sample Solution

Transfer a 25-mL aliquot portion of the dilute Vitamin C sample solution into a 250-mL
Erlenmeyer flask and add 25 mL aliquot of the I2 solution. Important: The mixture must turn to
brown. If the solution remains colorless then increase the volume of the I2 solution or by
decrease the volume of the dilute Vitamin C sample solution. Consult your lab instructor.
Titrate with 0.1 M Na2S2O3 until the color of the mixture turns to lemon yellow. Add 1 mL of
the starch indicator and continue titrating with 0.1 M Na2S2O3 until the blue color disappears.
Perform 3 trials. Note: The presence of the starch in the tablet may cause the solution to turn
to dark green or blue. If this happens, there is no need to add starch.

Report the composition of the Vitamin C tablet in terms of mg ascorbic acid/tablet.

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 A Compilation of Experiments and Procedures for Analytical Chemistry Lab1
Experiment 57
Complexation Reaction: Determination of Ca in Drugs

Discussion:
Complexometric titrations have been carried out successfully on nearly all-common cations. These
reactions virtually replaced the former tedious gravimetric analyses for many metals in a variety of
samples. The most popular complexing agent is the EDTA (or H4Y, ethylenediaminetetraacetic acid). It
reacts with metal ions on a 1:1 stoichiometric mole ration.
For convenience, the free acid form of EDTA is often abbreviated as H4Y and the EDTA anion as
Y4-. Eriochrome Black T (EBT) is usually represented in abbreviated form as a tri basic acid, HIn3. An
NH3-NH4Cl buffer of pH 9 to 10 is often used for the metals that form complexes with ammonia. At pH
10, the predominant form of Eriochrome Black T is the blue HIn2 form. The reaction that results in the
color change can be written as
MIn- + HY2 MY2 + HIn2
(red) (blue)

In order for the color change to occur at the proper time, the stability of MIn- complex must be less
than that of MY2 so that the metal M releases the indicator when only a slight excess of EDTA is added.

If the sample titrated does not contain Mg, some Mg salt can be added to EDTA before this
solution is standardized. The titrant then (pH 10) is a mixture of MgY2 and Y4-. As this is added to the
solution containing Ca2+, the more stable CaY2 is formed, liberating Mg2+ to react with the indicator and
form the red MgIn-. After the calcium has been used up, additional titrant convenrts MgIn- to MgY2- and
the indicator reverts to the blue HIn2 form.

The complex formed between calcium ion and Eriochrome Black T is not very stable and the color
change occurs prematurely in the titration of Ca2+ with EDTA. Standardizing the EDTA solution against
standard calcium ion solution using conditions identical to those used for the unknown can reduce the
titration error. However, magnesium forms a stronger complex with the indicator than calcium and a
proper end point is obtained in an ammonia buffer of pH 10.

The total hardness of water due to calcium and magnesium ions can be determined by direct
titration with H4Y (ethylenediaminetetraacetic acid) using Eriochrome Black T or calmagite indicator.
The structure of the H4EDTA and the anionic form at pH 10 of the ligand is

HOOCH2C CH2COOH -
OOCH2C CH2COO
-
NCH2CH2N NCH2CH2N
- -
HOOCH2C CH2COOH OOCH2C CH2COO
-4 -4
H4EDTA (or H4Y) EDTA (or Y )

The EDTA anion is potentially a hexadentate ligand, which may coordinate with a metal ion through its
two nitrogens and four carboxylate groups.

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 A Compilation of Experiments and Procedures for Analytical Chemistry Lab1
Reaction with Metal Ions (at pH 10)
Ca2+ + HY3- CaY2- + H+
2+
Mg + HY3- MgY2- + H+

Reaction with Indicator:

Mg2+ + HIn2 MgIn- + H+
Ca2+ + MgIn CaIn- + Mg2+

Experimental Procedure:
1. Preparation of 0.01M EDTA solution:
Transfer about 2-g of disodium dihydrogen EDTA dihydrate and 0.1-g of MgCl2·6H2O into a
clean 400-ml beaker and dissolve the solids in water. If the solution appears turbid, add NaOH
solution until the solution is clear. Transfer the solution into an amber bottle, add enough distilled
water to make about 0.50 L and mix thoroughly. Label the contents of the bottle as 0.01 M EDTA.

2. Standardization of 0.01M EDTA solution using CaCO3

Prepare a calcium standard solution as follows: Accurately weigh about 0.2-0.4-g of primary
standard calcium carbonate that has been previously dried at 100oC. Transfer the solid to a 250-ml
volumetric flask, using about 100-ml water. Add 1:1 HCl dropwise until effervescence ceases and
the solution is clear. Dilute with water to the mark and mix solution thoroughly.
Pipet a 25-ml portion of the calcium standard solution into a 250-ml Erlenmeyer flask and add
5-ml of the ammonia-ammonium chloride buffer solution; then add 5 drops of Eriochrome Black T
indicator. Titrate carefully with the EDTA solution to the point where the color changes from wine-
red to pure blue. No tinge of red should remain in the solution. Repeat the titration with other
aliquots of calcium solution.

Report the concentration of the EDTA solution in terms of molarity and the Ca titer (mg Ca /mL
solution).

3. Determination of Ca in Drugs
The Lab Instructor will provide you with an OTC drug sample that contains calcium lactate only
and the some information regarding the composition of the drug. From this data, you will make the
detailed procedure for the determination of Ca in the drug sample. Based on your proposal, the
volume of the titrant that will be consumed for each analysis must lie within the range of 10 to 40
mL. Show the calculations to your Lab Instructor before proceeding.
Measure about 50 mL of distilled water into a 250-mL beaker and dissolve one or more tablets.
If the sample is not very soluble in distilled H2O, add about 5 mL of 0.5 M HCl and this will improve
its solubility. Transfer the dissolved tablet into a volumetric flask and dilute to the mark. Label the
mixture as dilute tablet solution (DTS). Determine the volume of the aliquot portion of the DTS that
must be measured so that
With the use of a volumetric pipet, obtain an aliquot portion of the DTS and transfer it into a 250-
ml Erlenmeyer flask. To the first sample add 1.0 ml of the buffer solution and 5 drops of the
indicator solution. Titrate with the standard EDTA solution to a color change of wine-red to pure-
blue. Perform the titration in triplicate measurements.

Report the composition of the sample in terms of value indicated in the label of the supplement, i.e.
as mg calcium lactate, Ca(CH3CH(OH)CO2)2, per tablet for Ca supplements or mg Ca per tablet.

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 A Compilation of Experiments and Procedures for Analytical Chemistry Lab1
Experiment 98
Optical Methods of Analysis: Determination of Mn in Solutions
See Canvas for Labster Simulation
Discussion:
All forms of matter interact with electromagnetic radiation (emr). When a molecule is exposed
to emr, it immediately absorbs the photon of energy and the electrons are promoted to an excited state.
For polyatomic substances, the transition can involve a change in the electronic, vibration or rotational
state.
A plot of the absorbance of the solution containing the absorbing species as a function of the
wavelength is a broad spectrum called the absorption spectrum. The broad bank of the absorption
spectrum is due to the large number of vibrational and rotational energy levels that are closely spaced
and are not independently distinguishable. The wavelength of greatest absorption ( max) corresponds
to the transition that will occur with the highest probability and that which involves the most number of
molecules.
The mathematical relationship between absorbance, A, and concentration, c, is expressed by the
Beer s Law: A = abc

The absorbance of a solution is equal to the product to the molar absorptivity, a, the cell path
length of the container and the concentration of the absorbing species. The application of Beer s law to
the quantitative analysis is broad. The information that can be obtained varies from the source of the
electromagnetic radiation, physical state of the absorbing species and the ability of the instrument to
isolate the emr absorbed or emitted by the absorbing species.

Experimental Procedure
1. Preparation of the Standard Solution
Prepare 250 mL of 0.01 M MnSO4 standard solution from MnSO4·H2O.
Transfer 10.0 mL of the 0.01 M MnSO4 solution into a a250-mL beaker and add about 100
mL of distilled water. Add 10 mL 85%H3PO4 and 0.5 g KIO4. Heat the mixture gently and allow
the solution to boil for about 3 minutes. The color of the mixture will change to purple. Allow the
solution to cool and transfer the contents quantitatively to a 250-mL volumetric flask. Rinse the
beaker with about three 20-mL portions of distilled H2O. Transfer the rinsing into the volumetric
flask. Dilute to the mark with distilled H2O and cover. Mix the solution thoroughly. Label the
solution

Calculate the concentration of permanganate standard solution (PSS). Express your answer in
terms of the moles Mn per Liter of solution.

2. The Absorption Spectrum and Working Wavelength

Measure the absorbance of the permanganate standard solution (PSS) prepared in number 1
at various wavelength values. Cover the range from about 440 nm to 720 nm. Record the readings
every 20 nm.
Plot the absorbance (y-axis) versus the wavelength (x-axis). Identify the region of maximum
absorbance. This is the proper wavelength to use for the measurement of the absorbance of the Mn
solution at different concentrations. The wavelength at which the absorbance is greatest is referred
to as the working wavelength. All succeeding absorbance measurements must be done at this
wavelength.

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3. Standard Calibration Curve:

Obtain 4 clean 50-mL volumetric flasks and label each one from numbers 1 to 5. Measure
accurately 10, 20, 30 and 40 mL of the PSS and transfer into flasks labeled 1, 2, 3, 4 respectively.
Dilute to the mark with distilled H2O. Cover the flask securely and mix the solution thoroughly.
Use the PSS (do not dilute) as standard solution 5.

Flask Volume (mL) of PSS Added Standard Solution (SS)

1 10 1
2 20 2
3 30 3
4 40 4

Calculate the molar concentration of Mn present in each of the five standard solutions.

4. Beer s Law
Note: Perform this portion of the experiment only when the sample is ready.
Adjust the wavelength setting of the Spectronic 20 to the working wavelength. With distilled H2O
as the blank, set the absorbance of the blank (distilled H2O) to zero. Measure the absorbance of the
five standard solutions. Do 3 readings for every standard solution. Beer s Law is obeyed if the
absorbance reading increases with increasing concentration of the standard solution.

Calculate the average absorbance of each standard solution. Plot the absorbance (y-axis) versus the
concentration of the standard solution. Use the methods of least squares to determine the best straight
line for the data points. Report the equation of the line and the regression coeffient, r.

5. Analysis of Sample
C. Preparation of the Sample
Weigh the unknown sample and transfer into a 100 mL beaker. Add 50 mL of distilled H2O,
10 mL 85%H3PO4 and 0.5 g KIO4. Heat the mixture gently and allow the solution to boil for about
3 minutes. Allow the solution to cool and then transfer the colored solution into a 100-mL
volumetric flask. Rinse the beaker three times using 10-mL portions of distilled H2O. Transfer the
rinsing into the volumetric flask and dilute to the mark. Cover the flask and mix the solution
thoroughly. Label the solution as unknown solution (US)

D. Measurement of the Absorbance of the Unknown Solution

With the Spectronic 20 set at the working wavelength, measure the absorbance of the
unknown solution (US) after the absorbance of the five standard solutions were measured. The
absorbance of the unknown solution (US) must lie within the range of the absorbance of the five
standard solutions. It should not be lower than the absorbance of the SS1 nor should it be greater
than the absorbance of the SS5. Consult your Lab Instructor in case one of these cases happens to
your unknown solution.

Report the composition of the unknown sample in terms of %Mn.

Students are expected to generate their own Data Sheet for this experiment.

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