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Work Sheets for Analytical Chemistry Lab1

LBYCH27 WORKSHEETS
(ASA, D&C and Exercise
Sheets)

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Work Sheets for Analytical Chemistry Lab1

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.

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 is 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
a. observed using either direct perception (or direct method) using the eyes or indirect measurement
involves the use of an instrument
b. interpreted by the observer and recognize the change as a significant difference in a variable
property of the system
c. 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

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Work Sheets for Analytical Chemistry Lab1

A chemist seeks to establish a mathematical relationship between a property and what was 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.

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.

Errors in Chemical Analysis


Error is the difference between a measured value and the true value (the known or accepted value).

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 measurement to the true or “accepted true value”


Absolute error or Error, E = xi   where  is the true value
Note: Do not be misled by the word absolute. This does not refer to the operation absolute value.
 xi   
Relative error (%), ER =  100

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

Deviation, d = xi - x 

Relative deviation, =
xi  x x100
x

  xi  x 
2
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 =  1000
x

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Work Sheets for Analytical Chemistry Lab1
Exercise 1
Measurements and the Statistical Evaluation of Data

Materials and Glassware:


10-mL Volumetric Pipet Three 5--peso coins 3- 50-mL beakers
25 mL Volumetric Flask 250-mL beaker Funnel
Watch Glass Base Buret

Experimental Procedure
A. Measurement of Mass

1. Weighing by Addition (Note: Use an analytical balance)


Fill a clean 250-mL beaker with about 200 mL of distilled H2O.
Label each of the 3 clean and dry 50-mL beakers. Weigh the first beaker and record each value
correctly. Fill a clean volumetric pipet (10 mL capacity) with distilled H2O and drain it into the first
beaker. Measure the total mass of the beaker and distilled H2O and record the value under Trial 1.
Repeat the same procedure described above and record the values under Trial 2 and Trial 3.
Always be certain that the volume of the distilled H2O is constant for all 3 trials.

2. Weighing by Difference (Note: Use an analytical balance)


Reset the analytical balance to zero. Put all three 5-peso coins into the dry watch glass and record its
value. Remove one coin and record the total mass of the watch glass and the other two coins.
Remove the second coin and record the total mass of the watch glass and the remaining coin.
Remove the last coin and record the mass of the watch glass.

B. Measurement of Volume Capacity of Volumetric Flask

Weigh a dry 25--mL volumetric flask with stopper and record its value. Add enough distilled H2O until
the flask is filled to the mark. Wipe the flask and cover with the stopper. Weigh the flask filled with
distilled H2O.

Carefully empty the flask. Refill the flask with distilled water to the mark and tissue off the excess
water. Weigh the assembly and record the total mass under Trial 2. Repeat this procedure record the
measurement under Trial 3.

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Work Sheets for Analytical Chemistry Lab1

Group No. ID Number Date


Family Name

Given Name M.I.

Exercise 1
Measurements and the Statistical Evaluation of Data
Data & Calculation Sheet

A. Measurement of Mass
1. Weighing by Addition
Details Trial 1 Trial 2 Trial 3
Volume (mL) of Distilled H2O in Each Beaker 25.00 25.00 25.00
Temperature of the Distilled H2O (C) 23.0
Mass (g) of beaker plus Distilled H2O 53.7141 53.7102 53.7070
Mass (g) of empty beaker 29.0361 29.0358 29.0373
Mass (g) of Distilled H2O
Density of Distilled Water
Theoretical Value of the Density of distilled H 2O 0.997542
Average
Absolute Error
Relative Error (%)

2. Weighing by Difference
Details Trial 1 Details Trial 2 Details Trial 3
Mass (g) of Watch Mass (g) of Watch Mass (g) of Watch
45.5567 37.7254 29.9695
Glass plus 3 Coins Glass with 2 Coins Glass with 1 Coin
Mass (g) of Watch Mass (g) of Watch Mass (g) of Watch
37.7254 29.9695 22.2340
Glass plus 2 Coins Glass plus 1 Coin Glass
Mass (g) of Coin Mass (g) of Coin Mass (g) of Coin
Removed Removed Removed
Average Mass of Coin
Deviation Deviation Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Work Sheets for Analytical Chemistry Lab1

B. Measurement of Volume Capacity of Volumetric Flask

Details
Temperature of the Distilled H2O (C) 23.0
Theoretical Value of the Density of distilled H 2O 0.997542
Trial 1 Trial 2 Trial 3
Mass (g) of Volumetric Flask + Distilled H2O 43.8833 43.8836 43.8831
Mass (g) of dry Volumetric Flask 19.21670 19.2670 19.2666
Mass (g) of Distilled H2O
Volume (mL) of Distilled H2O in Volumetric Flask
Average Volume (mL) of Distilled H2O
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Work Sheets for Analytical Chemistry Lab1

Experiment 24
The Standardization of a Basic Solution and the
Determination of the Molar Mass of an Acid (Revised)

Materials and Glassware:


Brown bottle (about 1 L capacity) Funnel 100 mL beaker
Pipet (25-mL) Base Buret 10-mL graduated cylinder

Reagents and Solutions


Phenolphthalein Indicator Solution 0.1 M HCl Standard Solution 6 M NaOH Stock Solution

Experimental Procedure
A. Preparation and Standardization of 0.1 M NaOH.
1. Preparation of the NaOH Solution
Pour 100 mL of distilled water into a clean brown bottle. Measure 7 mL of 6 M NaOH stock
solution and transfer it into the brown bottle. Add about 300 mL more of distilled water into the brown
bottle and securely stopper the container. Shake and invert the solution several times to mix the
solution thoroughly. Do this several times in order to obtain a homogeneous solution. Initially label
the solution as 0.1 M NaOH and set aside.

2. Titration of the HCl Standard Solution with the Dilute NaOH Solution
Transfer about 100 mL of the dilute NaOH solution into a 250-mL beaker. Rinse the buret with
about 10 mL of the dilute NaOH solution. Drain the rinsing down the sink. Fill the buret with the dilute
solution. Open the pinch clamp to allow the solution to drain downwards and fill the air gap. Refill the
buret with the dilute NaOH. Record the initial buret reading. Important: The initial buret reading
need not be 0.00 mL and can be any value between 0 and 2 mL.
Measure 25 mL of the 0.1 M HCl standard solution with a pipet and transfer into an Erlenmeyer
flask. Add 50 mL of distilled water (use a graduated cylinder) to the flask, and 2 to 3 drops of the
indicator solution. Swirl the mixture and titrate with the dilute NaOH solution until the color of the
mixture in the flask changes in color from colorless to faint pink. Record the final buret reading. Pour
the mixture down the sink and flush with running water.
Perform 2 more trials using the same procedure described above.

B. Determination of the Molar Mass of an Unknown Monoprotic Acid, HA


Weigh the first sample of the unknown and record the mass on your notebook. Transfer the entire
amount into a clean Erlenmeyer flask labeled as trial 1. Weigh the empty container (either a vial or
weighing bottle) again in order to determine the mass of the unknown sample that was transferred
into flask. Dissolve the unknown sample in 50-75 mL of distilled water (use a 100-mL graduated
cylinder) and add 2 to 3 drops of the phenolphthalein indicator solution. Swirl the flask. Titrate the
dissolved unknown sample with the dilute NaOH solution until the phenolphthalein end point. Repeat
the analysis using the remaining two samples of the unknown acid.

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Work Sheets for Analytical Chemistry Lab1

Chem Notes:

Note 1: A standard solution is a solution whose concentration is accurately known. For example the
concentration of the HCl standard solution is reported as 0.1024 M.

Note 2: In this experiment, the accurate concentration of the NaOH solution is determined by titrating an
accurate amount of the HCl solution with NaOH solution until the phenolphthalein end point. The
HCl is referred to as the secondary standard.

Note 3: Take note of the number of divisions found for every 1 mL of the buret. Always report the volume
until 1/10th of the smallest known division.

Note 4: The mass of the unknown acid is obtained using the weighing technique referred to as weighing by
difference. The mass of the unknown acid is the difference between the initial mass and the final
mass.

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Work Sheets for Analytical Chemistry Lab1

Group No. ID Number Date


Family Name
Given Name M.I.

Exercise 2: Sample Data Calculation Sheet


Experiment 24 The Standardization of a Basic Solution and the
Determination of the Molar Mass of an Unknown Acid, HA

A. Standardization of NaOH Solution


Chemical Reactions: Molecular Equation: HCl(aq) + NaOH(aq)  NaCl(aq) + H2O(l)
Net Ionic Equation: H+(aq) + OH-(aq)  H2O(l)

Details Trial 1 Trial 2 Trial 3


Molarity of HCl Standard Solution 0.1024
Volume (mL) HCl Standard Solution 25.00 25.00 25.00
No. of mmoles HCl = No. of mmoles H+ _____________ _____________ _____________
No. of mmoles OH- reacted with HCl _____________ _____________ _____________
No. of mmoles NaOH reacted with HCl _____________ _____________ _____________
Final Reading (mL) NaOH Buret 22.17 22.15 22.28
Initial Reading (mL) NaOH Buret 0.05 0.05 0.10
Volume (mL) NaOH Solution Delivered _____________ _____________ _____________
Molarity of NaOH 0.1157 0.1158 0.1154
Average Molarity of NaOH
Deviation _____________ _____________ _____________
Standard Deviation _____________
Relative Standard Deviation (%) _____________

B. Determination of the Molar Mass of an Unknown Acid, HA


Chemical Reactions: Molecular Equation: HA(aq) + NaOH(aq)  NaA(aq) + H2O(l)
Net Ionic Equation: HA(aq) + OH-(aq)  H2O(l) + A-(aq)

Details Trial 1 Trial 2 Trial 3


Mass of container plus contents (g) 27.8792 28.7518 28.4300
Mass of container less contents (g) 27.4518 28.3217 28.0013
Mass (g) of Unknown sample Obtained _____________ _____________ _____________
Average Molarity of NaOH 0.1156 M
Initial Buret Reading (mL) 1.20 0.50 1.00
Final Buret Reading (mL) 19.30 18.67 19.27
Volume (mL) NaOH Delivered _____________ _____________ _____________
No. of mmol NaOH _____________ _____________ _____________
No. of Moles of Unknown Acid, HA ________ x 10-3 ________ x 10-3 ________ x 10-3
Molar Mass (g/mole) _____________ _____________ _____________
Average Molar Mass (g/mol) _____________
Deviation _____________ _____________ _____________
Standard Deviation _____________
Coefficient of Variation (%RSD) _____________

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Work Sheets for Analytical Chemistry Lab1

Group No. ID Number Date


Family Name
Given Name M.I.

Exercise 3: Sample Data Calculation Sheet


Experiment 28 Determination of Ascorbic Acid from an OTC Vitamin

Experimental Procedure.
Choose an over the counter (OTC) vitamin tablet that contains ascorbic acid. Weigh out 1 tablet of the vitamin
sample and transfer into a 100-mL beaker. Dissolve the tablet in distilled H2O dilute the mixture to 250-mL
using a volumetric flask. Obtain a 50-mL aliquot portion and titrate until the starch endpoint. Perform 3 trials.

A. Determination of Ascorbic Acid from an OTC Vitamin


Chemical Reactions: C6H8O6 (aq) + I2 (aq)  2I-(aq) + 2H+(aq) + C6H6O6 (aq)

Details
Preparation of Dilute Table Solution
Molarity of I2 Standard Solution 0.02512 M
Molar Mass (g/mole) Ascorbic Acid 176.14
Number of Tablets per Analysis 1
Mass (g) Container plus 1 Tablet 12.2546
Mass (g) Container less 1 Tablet 11.7824
Mass (g) of 1 Tablet 0.4722
Volume (mL) of Dilute Tablet Solution 250.00
Titrimetric Analysis of Dilute Tablet Trial 1 Trial 2 Trial 3
Solution
Volume (mL) of Aliquot Portion of
50.00 50.00 50.00
Dilute Tablet Solution Titrated
Final Buret Reading (mL) 11.64 22.80 11.20
Initial Buret Reading (mL) 0.20 11.64 0.00
Volume (mL) I2 Solution Delivered
No. of mmol I2 Reacted
No. of mmol Ascorbic Acid in Aliquot
Total No. of mmol Ascorbic Acid Present
in the Volumetric Flask
Total Mass (mg) of Ascorbic Acid
Present in 1 Tablet
Average Mass Ascorbic Acid/Tablet _____________ mg Ascorbic Acid/Tablet
Deviation
Standard Deviation
Coefficient of Variation (%RSD)
Reported Composition of Tablet 250 mg Ascorbic Acid /Tablet

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Work Sheets for Analytical Chemistry Lab1
Group No. ID Number Date
Family Name
Given Name M.I.

Experiment 1 Advanced Study Assignment


Analysis of an Impure Sample of Sodium Carbonate

1. The diequivalent base sodium carbonate is used as the primary standard in the standardization of a strong acid.
Titration of sodium carbonate with HCl to the methyl orange end point involves the reaction of 1 mole of Na 2CO3
with 2 moles of HCl. Write the balanced chemical equation in
a. molecular form

b. net ionic form

2. Standardization of a Basic Solution


A 0.1105 g sample of primary standard grade Na2CO3 (M.M. = 105.99) was dissolved in 55 mL of distilled H2O.
The solution required 22.18 mL of the HCl solution to reach the methyl orange end point.

a. Calculate the number of moles of primary standard grade Na 2CO3.

b. How many moles of HCl reacted with the Na2CO3?

c. Calculate the molarity of the HCl solution.

3. Analysis of an Impure Sample of Sodium Carbonate


A 0.3147 g sample containing Na2CO3 was dissolved in 60 mL of distilled H2O and 2-3 drops of methyl orange
were added to the mixture. The solution needed 38.73 mL of 0.1214 M HCl to reach the methyl orange end point.

a. Calculate the number of moles of HCl needed to reach the methyl orange end point.

b. How many moles of Na2CO3 reacted with the HCl?

c. Calculate the mass (g) of Na2CO3 present in the sample.

d. What is the %Na2CO3 present in the sample?

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Work Sheets for Analytical Chemistry Lab1

Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 1 Data & Calculations


Analysis of an Impure Sample of Sodium Carbonate

Table 1. Standardization of 0.1 M HCl Against the Primary Standard Sodium Carbonate, Na 2CO3
Balanced Chemical Equation:
Details Trial 1 Trial 2 Trial 3
Mass (g) Beaker plus Na2CO3
Mass (g) Beaker less Na2CO3
Mass (g) Na2CO3 obtained
Amount (moles) Na2CO3
Amount (moles) HCl reacted with Na2CO3
Final Buret Reading
Initial Buret reading
Volume (mL) of the HCl solution Delivered
Molarity of HCl solution
Average Molarity of HCl solution
Deviation
Standard Deviation
Coefficient of Variation (%RSD)
Table 2. Determination of Na2CO3 in an Impure Sample
Balanced Chemical Equation:
Details Trial 1 Trial 2 Trial 3
Mass (g) of packet plus sample
Mass (g) of packet less sample
Mass (g) sample
Average Molarity of HCl solution
Final Buret Reading
Initial Buret reading
Volume (mL) of the HCl Solution Delivered
Amount (moles) HCl needed to reach the end point
Amount (moles) Na2CO3 reacted with HCl
Mass (g) Na2CO3 present in the sample
Mass Percent Na2CO3, %(w/w) Na2CO3
Average %(w/w) Na2CO3
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

Group No. ID Number Date

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Work Sheets for Analytical Chemistry Lab1
Family Name
Given Name M.I.

Experiment 2 Advance Study Assignment


Determination of the Total Acidity of Vinegar

A. Acid Base Reaction


The compound potassium hydrogen phthalate, abbreviated as KHP, is a common primary standard used in the
standardization of a strong base titrant. It is a monoprotic acid and reacts on a 1:1 stoichiometric ratio with
NaOH.

2. Write the chemical formula of potassium hydrogen phthalate. _________________________

3. Draw the missing atoms to complete the structure of potassium hydrogen phthalate and encircle the acidic hydrogen.

B. Standardization of a Basic Solution


A 0.4047 g sample of primary standard grade potassium hydrogen phthalate (M.M. = 204.23) was dissolved
in distilled H2O. The solution required 22.42 mL of the NaOH solution to reach the phenolphthalein end
point.

3. Calculate the number of moles of KHP.

4. How many moles of NaOH will react with the KHP dissolved in water?

5. Calculate the molarity of the NaOH solution.

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Work Sheets for Analytical Chemistry Lab1

C. Analysis of Vinegar
A 25.00 mL vinegar sample was diluted to 250-mL using a volumetric flask. A 50.00 mL aliquot portion of
the dilute vinegar solution needed 35.45 mL of 0.1200 M NaOH to reach the phenolphthalein end point.

6. Calculate the number of moles of NaOH required to reach the endpoint.

7. Calculate the number of moles of acetic acid present in the 50-mL aliquot portion that was titrated.

8. Since the aliquot portion that was titrated was obtained from the dilute vinegar solution contained in the
volumetric flask. Then, the concentration of acetic acid in the aliquot portion is equal to the concentration of
acetic acid in the volumetric flask.

Concentration Acetic Acid (VF)  Concentration Acetic Acid Titrated (Aliquot Portion)

Total Amount (moles) Acetic acid VF Amount (moles) Acetic acid Aliquot Portion

Volume (mL) VF Volume (mL) Aliquot Portion

Therefore, the total amount (moles) acetic acid dissolved inside the solution contained in the volumetric flask is:

Amount (moles) Acetic acid Aliquot Portion


Total Amount (moles) Acetic acid VF   Volume (mL) VF
Volume (mL) Aliquot Portion

9. Calculate the total mass (g) of acetic acid dissolved in the solution contained in the volumetric flask (VF).

10. The mass (g) of acetic acid dissolved in the solution contained in the volumetric flask came from the 25.00 mL
vinegar sample. Calculate the %CH3COOH (w/v) present in the 25.00 mL vinegar sample.

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Work Sheets for Analytical Chemistry Lab1

Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 2 Data & Calculations


Determination of the Total Acidity of Vinegar

Table 1. Standardization of 0.1 M NaOH Against the Primary Standard


Potassium Hydrogen Phthalate (KHC8H4O4)
Balanced Chemical Equation

Details Trial 1 Trial 2 Trial 3


Mass (g) of container plus KHC8H4O4
Mass (g) container less KHC8H4O4
Mass (g) KHC8H4O4
Amount (moles) KHC8H4O4
Amount (moles) NaOH reacted with KHC8H4O4
Final Buret Reading
Initial Buret reading
Volume (mL) of the NaOH Solution Delivered
Molarity of NaOH solution
Average Molarity of NaOH Solution
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Work Sheets for Analytical Chemistry Lab1

Table 2. Determination of Acetic Acid in Vinegar


Balanced Chemical Equation

Details Trial 1 Trial 2 Trial 3


A. Preparation of the Dilute Sample Solution
Volume (mL) of Vinegar Sample 25.00
Volume (mL) of Dilute Sample Solution 250.00
B. Titrimetric Analysis of the Dilute Sample Solution (DSS)
Volume (mL) of DSS Titrated 25.00 25.00 25.00
Average Molarity of NaOH solution
Final Buret Reading
Initial Buret reading
Volume (mL) of the NaOH Solution Delivered
Amount (moles) NaOH needed to reach the end point
Amount (moles) CH3COOH in Aliquot Portion
Molarity of CH3COOH in Aliquot Portion
Molarity of CH3COOH in the VF
Total Amount (moles) CH3COOH in the prepared DSS
Total Mass (g) ) CH3COOH
% (w/v) CH3COOH in the Vinegar Sample
Average %(w/v) CH3COOH
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Work Sheets for Analytical Chemistry Lab1

ID
Group No. Date
Number
Family Name
Given Name M.I.

Experiment 3 Advance Study Assignment


Titration Curve: Strong Acid-Strong Base Reaction

The titration reaction between a strong acid and a strong base is monitored by measuring the pH of the titration mixture
after each addition of 1.00 mL of the titrant. A 25.00 mL solution of a strong acid was titrated with 0.1020 M NaOH
solution. The titration curve is given below:
Titration Curve: Strong Acid-Strong Base Reaction

14.00

12.00

10.00

8.00

6.00

4.00

2.00

0.00
0.00 5.00 10.00 15.00 20.00 25.00 30.00 35.00
Volume (mL) NaOH

1. From the titration curve, show how the equivalence point is determined.
2. How many milliliters of the titrant are needed to reach the equivalence point? ________ mL
3. Based on the value reported in number 2, calculate the concentration of the strong acid.

4. The transition in color for phenol red is 6.8 – 8.4 while that of phenolphthalein is from 8.3 to 10.0. On the titration
curve, indicate the pH range where the transition occurs for both indicators. Explain briefly which is better to use as
indicator for the reaction between a strong acid and a strong base.

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Work Sheets for Analytical Chemistry Lab1

Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 3 Data and Calculations Sheet


Titration Curve: Strong Acid-Strong Base Reaction

Table 1. Titrimetric Analysis of an Unknown Strong Acid (HCl) Solution


Balanced Chemical Equation:
Details Trial 1 Trial 2 Trial 3
A. Preparation of the Dilute Unknown Solution (DUS)
Volume (mL) of Original Unknown Solution
Volume (mL) of Dilute Unknown Solution
B. Titrimetric Analysis of the Dilute Unknown Solution (DUS)
Volume (mL) of DUS Titrated
Average Molarity of NaOH solution
Final Buret Reading
Initial Buret reading
Volume (mL) of the NaOH Solution Delivered
Amount (mmoles) NaOH needed to reach the end point
Amount (mmoles) HCl
Molarity of Dilute Unknown HCl Solution
Molarity of Original Unknown Solution of HCl
Average Molarity of Original Unknown Solution of HCl
Deviation
Standard Deviation
Coefficient of Variation (%RSD)
C. Potentiometric Titration of the Dilute Unknown Solution (DUS)
Volume (mL) of DUS Titrated
Average Molarity of NaOH solution
Volume (mL) of the NaOH Solution Needed to reach the
Graphical End Point
Amount (mmoles) NaOH needed to reach the end point
Amount (mmoles) HCl
Molarity of Dilute Unknown HCl Solution
Molarity of Original Unknown Solution of HCl

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Work Sheets for Analytical Chemistry Lab1

ID
Group No. Date
Number
Family Name
Given Name M.I.

Experiment 4 Advanced Study Assignment


Determination of the Dissociation Constant of a Weak Acid

1. The pH of a 0.120 M CH3COOH ( Ka = 1.75 x 10-5) is ______________.

2. The pH of a 0.120 M NaCH3CO2 is ______________.

3. Consider the reaction between 25.00 mL of 0.120 M CH3COOH with 15.00 mL of 0.120 M NaOH.
a. How many mmol of CH3COOH are dissolved in 25.00 mL of 0.120 M CH3COOH?

b. How many mmol of NaOH are dissolved in 15.00 mL of 0.120 M NaOH?

c. The limiting reactant is _________________ while the excess reactant is ________________.

d. After adding the 25.00 mL solution of the weak acid and the 15.00 mL solution of the strong base together, the

total volume of the mixture is ____________ mL.

e. How many mmol of NaCH3CO2 will be obtained from the reaction?

f. What is the molar concentration of NaCH3COO?

g. How many mmol of CH3COOH will be remain unreacted or is in excess?

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Work Sheets for Analytical Chemistry Lab1
h. What is the molar concentration of CH3COOH?

i. The mixture contains the weak acid, acetic acid and its conjugate base, acetate ion. The acid to base ratio is

 weak acid  
 CH COOH  
3

 conjugate base CH CO 


3

2
__________________ =

j. The pH of the solution is _____________.

4. Consider the reaction between 25.00 mL of 0.120 M CH3COOH with 25.00 mL of 0.120 M NaOH.
a. How many mmol of CH3COOH are dissolved in 25.00 mL of 0.120 M CH3COOH?

b. How many mmol of NaOH are dissolved in 25.00 mL of 0.120 M NaOH?

c. How many mmol of NaCH3CO2 will be obtained from the reaction?

d. What is the molar concentration of NaCH3COO?

e. The pH of the solution when only the product sodium acetate is present in the solution.

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Work Sheets for Analytical Chemistry Lab1

Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 4 Data & Calculations


Determination of the Dissociation Constant of a Weak MonoproticAcid

Table 1. Titrimetric Analysis of an Unknown Solution of a Weak Monoprotic Acid, HA


Balanced Chemical Equation:
Details Trial 1 Trial 2 Trial 3
A. Preparation of the Dilute Unknown Acid (HA) Solution (DUS)
Volume (mL) of Original Unknown Acid (HA) Solution
Volume (mL) of Dilute Unknown Acid (HA) Solution
B. Titrimetric Analysis of the Dilute Unknown Acid Solution (DUS)
Volume (mL) of DUS Titrated

Average Molarity of NaOH solution

Final Buret Reading


Initial Buret reading
Volume (mL) of the NaOH Solution Delivered
Average Volume (mL) of NaOH Needed to Reach End Point
The pH Reading of Titration Mixture at End Point
Amount (mmoles) NaOH needed to reach the end point
Amount (mmoles) HA
Molarity of Dilute Unknown Acid Solution (DUS)
Molarity of Original Unknown Acid (HA) Solution
Average Molarity of Original Unknown Acid (HA) Solution
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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C. Titration at Midpoint
Volume (mL) of DUS Titrated

Volume (mL) of the NaOH Solution to Midpoint


The pH Reading at Midpoint
The pKa of the Weak Acid
The Acid Dissociation Constant, Ka of the
Monoprotic Acid, HA
Average Acid Dissociation Constant, Ka
D. Potentiometric Titration of the Dilute Unknown Acid Solution (DUS)
Volume (mL) of DUS Titrated

Average Molarity of NaOH solution


Volume (mL) of the NaOH Solution Needed to reach the
Graphical End Point
Amount (mmoles) NaOH needed to reach the end point
Amount (mmoles) HA
Molarity of Dilute Unknown HA Solution
Molarity of Original Unknown Solution of HA
E. Graphical Determination of the Acid Dissociation Constant
Volume (mL) of of the NaOH Solution
Needed to Reach the Midpoint of the Titration Curve
The pH at the Midpoint
The pKa of the Weak Acid
The Acid Dissociation Constant, Ka of the
Monoprotic Acid, HA

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Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 5 Advance Study Assignment


Preparation of Buffers

Write the balanced chemical equation that will represent the hydrolysis of the acidic and basic salts that were analyzed.
1. When dissolved in water, sodium acetate, NaCH3CO2, dissociates to form Na+ and CH3CO2- ions.
Write the chemical equation that will represent the complete dissociation of sodium acetate in water.

Write the balanced chemical equation that will represent the hydrolysis of acetate ion.

What ion is released from the hydrolysis that proves the basic nature of the acetate ion in aqueous solutions?

2. When dissolved in water, ammonium nitrate, NH4NO3, dissociates to form NH4+ and NO3- ions.
Write the chemical equation that will represent the complete dissociation of ammonium nitrate in water.

Write the balanced chemical equation that will represent the hydrolysis of ammonium ion.

What ion is released from the hydrolysis that proves the acidic nature of the ammonium ion in aqueous solutions?

3. Is there a difference between the pH of the solution for NaCl and KNO 3? ____________
General Trend Observed: All neutral salts have a pH of _________________.

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4. Complete the table below:

Description of Aqueous Solution of


Dissociation Products
the Salt
Salt
Acidic, Basic or pH
Cation Anion
Neutral (Check the answer)
pH < 7
NaBr pH = 7
pH > 7
pH < 7
KNO3 pH = 7
pH > 7
pH < 7
NaCH3CO2 pH = 7
pH > 7
pH < 7
NH4Cl pH = 7
pH > 7

5. Consider the following solutions listed below and write a check on the space after the mixtures that will produce a
buffer
0.10 M HCl 0.10 M CH3COOH 0.10 M NH4Cl 0.10 M Na2HPO4
0.10 M NaOH 0.10 M H3PO4 0.10 M NH3 0.10 M NaH2PO4

a. 25 mL of 0.10 M HCl and 25 mL of 0.10 M NaOH _____________________

b. 25 mL of 0.10 M HCl and 25 mL of 0.10 M NH3 _____________________

c. 25 mL of 0.10 M HCl and 25 mL of 0.10 M CH3COOH _____________________

d. 25 mL of 0.10 M NaOH and 25 mL of 0.10 M NH3 _____________________

e. 20 mL of 0.10 M HCl and 30 mL of 0.10 M NH3 _____________________

f. 20 mL of 0.10 M NaOH and 30 mL of 0.10 M CH3COOH _____________________

g. 20 mL of 0.10 M NaCH3CO2 and 30 mL of 0.10 M CH3COOH _____________________

h. 20 mL of 0.10 M NH4Cl and 30 mL of 0.10 M NH3 _____________________

i. 20 mL of 0.10 M NaH2PO4 and 30 mL of 0.10 M Na2HPO4 _____________________

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Family Name
Given Name M.I.

Experiment 5 Data & Calculations


Preparation of Buffers

Table 1. Measurement of the pH of Solutions


0.10 M Solution pH Reading 0.10 M Solution pH Reading 0.10 M Solution pH Reading
HCl HNO3 NaCH3CO2
NaOH NaNO3 NH3
NaCl CH3COOH NH4Cl

Table 2. Measurement of pH of Buffers


Composition
Mixture 0.1 M Acid Volume 0.1 M Base Volume (mL) Volume pH
Solution (mL) Acid Solution Base (mL) H2O
1 CH3COOH 20.00 NaCH3CO2 20.00 10.00
2 CH3COOH 20.00 NaOH 10.00 20.00
3 HCl 10.00 NaCH3CO2 20.00 20.00
4 NH4NO3 20.00 NH3 20.00 10.00
5 HNO3 10.00 NH3 20.00 20.00
6 NH4NO3 20.00 NaOH 10.00 20.00

Based on the results summarized in Table 2, identify if the conditions necessary to prepare buffers are met for each
mixture
Weak Acid to
No. of mole No. of mole
Acid Base Conjugate Base Ratio (pKa1) to (pKa1)
Before Mixing Before Mixing
(After Mixing)
CH3COOH NaCH3CO2
CH3COOH NaOH
HCl NaCH3CO2
NH4NO3 NH3
HNO3 NH3
NH4NO3 NaOH

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Given Name M.I.

Experiment 6 Advance Study Assignment


Determination of Ca in Drugs

Preparation of the Ca2+ standard solution


A 0.1104 g sample of primary standard grade CaCO3 (M.M. = 100.09) was transferred to a 100 mL beaker
containing 50-mL distilled H2O. Concentrated HCl was added to the mixture until clear. The solution was
transferred quantitatively to the 250-mL volumetric flask and diluted to the mark. Cover securely and mix the
solution thoroughly.

1. The molarity of the Ca2+ ions in the standard solution is ___________________________.

Standardization of a Solution
A 50-mL aliquot of the 0.04412 M Ca2+ standard solution was transferred into a conical flask. After adding 50 mL
H2O, the mixture needed 20.62 mL EDTA solution to reach the endpoint.

2. Calculate the molar concentration of the EDTA solution. ______________________ M EDTA

3. Express the concentration of the EDTA solution in terms of mg Ca/mL.


Calculate the amount (mmoles) Ca in the 50-mL aliquot.

Convert the amount (mmoles) Ca to mass (mg) Ca (M.M. = 40.08)

Divide the mass (mg) Ca by the volume of EDTA solution.

The ratio (mg Ca/mL) is the concentration of the EDTA solution expressed as Ca titer of EDTA.

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Analysis of Ca Supplement Drug

The composition of an OTC Ca Supplement is advertised as 325 mg calcium lactate, Ca(CH 3CH(OH)CO2)2 per tablet.
List of Molar Mass: Ca(CH3CH(OH)CO2)2 = 218.24; Ca = 40.08
4. Calculate the number of mmoles of Ca present in 1 tablet. ___________ mmol

5. How many mL of 0.0100 M EDTA solution will be needed to titrate a solution that contains 1 dissolved tablet of the
Ca supplement drug? ___________ mL

6. Would you recommend diluting the sample before titration? ___________


Support your answer.

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Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 6 Data & Calculations


Complexation Reaction: Determination of Ca in Drugs

Table 1. Standardization of 0.01 M EDTA Against the Primary Standard Calcium Carbonate
Balanced Chemical Equation:
Details Trial 1 Trial 2 Trial 3
2+
A. Preparation of Ca Standard Solution
Mass (g) of container plus CaCO3
Mass (g) container less CaCO3
Mass (g) CaCO3
Amount (mmoles) Ca = Amount (mmoles) CaCO3
Volume (mL) of Ca Standard Solution
Molarity of Ca Standard Solution
B. Determination of the Concentration of EDTA Solution (Molarity)
Balanced Chemical Equation
Molarity of Ca Standard Solution
Volume (mL) of Ca Standard Solution Titrated 25.00 25.00 25.00
Amount (mmoles) Ca
Amount (mmoles) EDTA reacted
Final Buret Reading
Initial Buret reading
Volume (mL) of the EDTA Solution delivered
Molarity of EDTA solution
Average Molarity EDTA solution
Deviation
Standard Deviation
Coefficient of Variation (%RSD)
C. Other Expressions of Concentration of the EDTA Solution
Average Molarity of EDTA Standard Solution
Ca titer (mg Ca/mL of EDTA solution)

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Table 2. Determination of Ca in Drugs


Balanced Chemical Equation
Details Trial 1 Trial 2 Trial 3
A. Preparation of the Dilute Tablet Solution
Number of Tablets Dissolved
Volume (mL) of Dilute Tablet Solution Prepared
B. Titrimetric Analysis of the Dilute Tablet Solution (DTS)
Volume (mL) of DTS Titrated

Average Molarity of EDTA Solution

Ca titer (mg Ca/mL of EDTA solution)

Final Buret Reading


Initial Buret reading
Volume (mL) of the EDTA Solution Delivered

C. Evaluation of the Drug


Option 1: Mass (mg) calcium lactate/tablet

Average Molarity of EDTA Solution


Volume (mL) of the EDTA Solution Delivered
Amount (mmoles) Calcium lactate present in the DTS Titrated
Total Amount (mmoles) Calcium Lactate
Mass (mg) Calcium Lactate / tablet
Average Mass (mg) of Calcium lactate/tablet
Reported Concentration of the Supplement Drug on Label
Deviation
Standard Deviation
Coefficient of Variation (%RSD)
Option 2: Report the Analysis in terms of Mass (mg) Ca present / tablet

Average Ca Titer of EDTA Solution (mg Ca/mL solution)


Volume (mL) of the EDTA Solution Delivered
Amount (mmoles) Ca present in the DTS Titrated
Total Amount (mmoles) Ca present
Mass (mg) Calcium / tablet
Average Mass (mg) of Ca/tablet
Reported Concentration of the Supplement Drug on Label

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Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 7 Advance Study Assignment


Determination of Hydrogen Peroxide
The aqueous solution of potassium permanganate, KMnO4 is a popular oxidant for redox reactions because it is a strong
oxidizing agent and titration with KMnO4 does not require the addition of an indicator solution. It acts as a self-indicator.
In acidic medium, the purple permanganate ion changes to the almost colorless Mn 2+ ion (pale pink ion).

1. Write the reduction half reaction of MnO4- in acidic medium.

2. Aside from pure iron metal, the solution of KMnO 4 is can also standardized using any one of the primary standards
Na2C2O4, H2C2O4·2H2O, KHC2O4·H2O, KHC2O4·H2C2O4·2H2O (commonly referred to as potassium tetroxalate).
Write the oxidation half reaction of oxalate ion, C 2O42-, in acidic medium (exists as H2C2O4)

3. Write the balanced reduction half-reaction and indicate the standard reduction potential when
a. hydrogen peroxide is reduced to water

b. O2(g) is reduced to hydrogen peroxide

Standardization of a KMnO4 Solution


A 0.2028 g sample of primary standard grade Na2C2O4 (M.M. = 134.00) was dissolved in 100 mL of 1 M
H2SO4. The solution required 22.42 mL of the KMnO4 solution to reach the phenolphthalein end point.
Titration of the blank (100 mL of 1M H2SO4) required 0.02 mL of the KMnO4 solution.

4. Calculate the number of mmoles of Na2C2O4.

5. Calculate the molarity of the KMnO4 solution.

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Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 7: Data & Calculations


Titrations with KMnO4

Table 1. Standardization of 0.02 M KMnO4 Against the Primary Standard Sodium Oxalate
Balanced Chemical Equation:

Details Trial 1 Trial 2 Trial 3


Mass (g) of container plus Na2C2O4
Mass (g) container less Na2C2O4
Mass (g) Na2C2O4
Amount (mmoles) Na2C2O4
Amount (mmoles) KMnO4 reacted with Na2C2O4
Final Buret Reading
Initial Buret reading
Volume (mL) of the KMnO4 Solution Delivered
Molarity of KMnO4 Solution
Average Molarity of KMnO4 Solution
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Table 2. Analysis of an Impure Sample of Ferrous Ammonium Sulfate Hexahydrate


Balanced Chemical Equation:

Details Trial 1 Trial 2 Trial 3


Mass (g) of packet plus sample
Mass (g) of packet less sample
Mass (g) sample
Average Molarity of KMnO4 solution
Final Buret Reading
Initial Buret reading
Volume (mL) of the KMnO4 Solution Delivered
Amount (mmoles) KMnO4 needed to reach the end point
Amount (mmoles) Fe2+ reacted with KMnO4
Amount (mmoles) Fe(NH4)2(SO4)26H2O
Mass (g) Fe(NH4)2(SO4)26H2O present in the sample
Mass Percent Fe(NH4)2(SO4)26H2O,
%Fe(NH4)2(SO4)26H2O
Average %Fe(NH4)2(SO4)26H2O
Deviation
Standard Deviation
Coefficient of Variation (%RSD)
Table 3. Determination of H2O2 in a Commercial Sample
Balanced Chemical Equation:

Details Trial 1 Trial 2 Trial 3


A. Preparation of the Dilute Sample Solution
Volume (mL) of Liquid Commercial Sample 25.00
Volume (mL) of Dilute Sample Solution 500.00
B. Titrimetric Analysis of the Sample Solution
Volume (mL) of DSS Titrated 25.00 25.00 25.00
Average Molarity of KMnO4 solution
Final Buret Reading
Initial Buret reading
Volume (mL) of the KMnO4 Solution Delivered
Amount (mmoles) KMnO4 needed to reach the end point
Amount (mmoles) H2O2 present in the aliquot portion of DSS
Total Amount (mmoles) H2O2 dissolved in the entire DSS
Total Mass (g) H2O2 dissolved in the entire DSS
% (w/v) H2O2 in the Commercial Sample
Average %(w/v) H2O2
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

Group No. ID Number Date

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Family Name
Given Name M.I.

Experiment 8: Advance Study Assignment


Analysis of a Household Bleaching Agent

The indirect titration method called the iodometric technique is a 2-step reaction. The preliminary reaction involves the
addition of a large excess of KI is added to the oxidizing agent and this releases the I 2. The I2 is then titrated with a
standard solution of sodium thiosulfate.

1. Write the half reaction representing the transformation of IO 3- to I2 (acidic medium).

Reduction Half Reaction: ________________________________________

2. Write the half reaction representing the transformation of I - to I2.

Oxidation Half Reaction: _________________________________________

3. Write the titration reaction between I2 and Na2S2O3.

_______________________________________________________________

Standardization of a Solution
A 50.00 mL aliquot portion of 0.01020 M KIO3 solution was transferred into a conical flask. After adding 2.0 g
KI and 2 mL of 6M HCl, the mixture was titrated with 31.32 mL of the Na 2S2O3 solution to the starch end point.

4. Calculate the number of mmoles of IO3-. _________________ mmoles IO3-

5. How many mmoles of I2 was released after the addition of KI? __________________ mmoles I2

6. How many mmoles Na2S2O3 reacted with the I2 produced? _____________ mmoles Na2S2O3-

7. What is the molarity of the Na2S2O3 solution? _________________ M Na2S2O3

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8. Write the half reaction representing the transformation of OCl - (hypochlorite ion) to Cl-(chloride) in acidic medium.

Reduction Half Reaction: ________________________________________

9. Write the half reaction representing the transformation of l - (iodide ion) to I2 (iodine) in acidic medium.

Reduction Half Reaction: ________________________________________

Analysis of Household Bleaching Agent


The composition of a commercially available household bleaching agent is advertised as 5% (w/v) NaOCl.

10. Calculate the number of mmoles of NaOCl present in 50 mL of the bleaching agent. ___________ mmol

11. Calculate the number of mmoles of Na2S2O3 that will react with the I2 that is generated from the reactions of the KI
with the NaOCl present in 50-mL of the bleaching agent. ___________ mmol Na 2S2O3

12. How many mL of 0.1025 M Na2S2O3 are required to deliver this amount? ___________ mL

13. Would you recommend diluting the sample before titration? ___________

14. What is the effect of diluting the sample to the volume of the titrant that will be consumed?

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Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 8: Data and Calculations Sheet


Analysis of a Household Bleaching Agent

Table 1. Standardization of 0.1 M Na2S2O3 Against the Standard Solution of KIO3


Balanced Chemical Equation:
Preliminary Reaction:

Titration Reaction:

Details Trial 1 Trial 2 Trial 3


Mass (g) of container plus KIO3
Mass (g) container less KIO3
Mass (g) KIO3
Amount (mmoles) KIO3
Volume (mL) of KIO3 Standard Solution
Molarity of KIO3 Standard Solution
Volume (mL) of Aliquot Portion of KIO3 Standard Solution 25.00 25.00 25.00
Amount (mmoles) KIO3 in Aliquot Portion
Amount (mmoles) I2 produced
Final Buret Reading
Initial Buret reading
Volume (mL) of the Na2S2O3 Solution Delivered
Amount (mmoles) of Na2S2O3 reacted with I2
Molarity of Na2S2O3 solution
Average Molarity of Na2S2O3solution
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Table 2. Analysis of a Household Bleaching Agent


Balanced Chemical Equation:
Preliminary Reaction:

Titration Reaction:

Details Trial 1 Trial 2 Trial 3


A. Preparation of the Dilute Sample Solution
Volume (mL) of Liquid Commercial Sample
Volume (mL) of Dilute Sample Solution
B. Titrimetric Analysis of the Sample Solution
Volume (mL) of DSS Aliquot Portion Titrated
Average Molarity of Na2S2O3 Solution
Final Buret Reading
Initial Buret reading
Volume (mL) of the Na2S2O3 Solution Delivered
Amount (mmoles) Na2S2O3
Amount (mmoles) I2 present in the aliquot portion of DSS
Amount (mmoles) NaOCl in aliquot portion of DSS

% (w/w) NaOCl in the Commercial Sample


Average %(w/w) NaOCl
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

Amount (mmoles) NaOCl in aliquot portion of DSS


% (w/v) NaOCl in the Commercial Sample
Average %(w/v) NaOCl
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Table 3. Analysis of a Household Bleaching Agent


Balanced Chemical Equation:
Preliminary Reaction:

Titration Reaction:

Details Trial 1 Trial 2 Trial 3


A. Preparation of the Dilute Sample Solution
Volume (mL) of Liquid Commercial Sample
Volume (mL) of Dilute Sample Solution
B. Titrimetric Analysis of the Sample Solution
Volume (mL) of DSS Aliquot Portion Titrated
Average Molarity of Na2S2O3 Solution
Final Buret Reading
Initial Buret reading
Volume (mL) of the Na2S2O3 Solution Delivered
Amount (mmoles) Na2S2O3
Amount (mmoles) I2 present in the aliquot portion of DSS

Amount (mmoles) Ca(OCl)2 in aliquot portion of DSS


% (w/w) Ca(OCl)2 in the Commercial Sample
Average %(w/w) Ca(OCl)2
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

% (w/v) Ca(OCl)2 in the Commercial Sample


Average %(w/v) Ca(OCl)2
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 9: Advanced Study Assignment


Analysis of Vitamin C

Iodimetric titration is the direct titration with I 2 solution. I2 is a weak oxidizing agent and is used to titrate strong
reductants.

1. Before the equivalence point, the addition of small amounts of the titrant, I 2, transforms it to the colorless iodide ion,
I-. After the equivalence point, there is a slight excess of the I 2 solution. In the presence of the starch indicator, what
color change happens to the mixture? _________________________________

2. Write the net redox reaction representing the reaction between ascorbic acid, C 6H8O6, and I2.

__________________________________________________________________________

Standardization of a Solution
A 25.00 mL aliquot portion of 0.02420 M C6H8O6 standard solution was transferred into a conical flask. After
adding 50 mL H2O, the mixture needed 26.12 mL I2 solution to reach the endpoint.

3. Calculate the number of mmoles of C6H8O6-. ______________ mmoles C6H8O6

4. How many mmoles of I2 reacted with the C6H8O6? __________________ mmoles I2

5. What is the molarity of the I2 solution? _________________ M I2

Analysis of Vitamin C Supplement


The composition of an OTC Vitamin C Supplement is advertised as 350 mg ascorbic acid per tablet.
6. Calculate the number of mmoles of C6H8O6 present in 1 tablet. ________________ mmol

7. How many mL of 0.025 M I2 solution will be needed to titrate a solution that contains 1 dissolved tablet of the OTC
drug? _________________ mL

8. Would you recommend diluting the sample before titration? _________________

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Group No. ID Number Date


Family Name
Given Name M.I.

Experiment 9: Data & Calculations


Analysis of Vitamin C

Table 1. Standardization of 0.025 M I2 Against the Standard Solution of Ascorbic Acid


Balanced Chemical Equation
Details Trial 1 Trial 2 Trial 3
Mass (g) of container plus Ascorbic Acid
Mass (g) container less Ascorbic Acid
Mass (g) Ascorbic Acid (C6H8O6)

Amount (mmoles) C6H8O6

Volume (mL) of C6H8O6Standard Solution

Molarity of C6H8O6 Standard Solution


25.00 25.00 25.00
Volume (mL) of Aliquot Portion of C6H8O6 Standard Solution

Amount (mmoles) C6H8O6 in Aliquot Portion

Final Buret Reading


Initial Buret reading
Volume (mL) of the I2 Solution Delivered
Amount (mmoles) of I2
Molarity of I2 solution
Average Molarity of I2 solution
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Table 2. Determination of Vitamin C in Drugs


Balanced Chemical Equation:
Addition Reaction:

Back-Titration Reaction:

Details Trial 1 Trial 2 Trial 3


A. Preparation of the Dilute Tablet Solution
Number of Tablets Dissolved
Volume (mL) of Dilute Sample Solution Prepared
B. Titrimetric Analysis of the Dilute Tablet Solution (DTS)
Volume (mL) of DTS Aliquot Portion

Average Molarity of I2 Solution

Volume (mL) of I2 solution added

Amount (mmoles) I2 added

Average Molarity of Na2S2O3 Solution

Final Buret Reading


Initial Buret reading
Volume (mL) of the Na2S2O3 Solution Delivered
Amount (mmoles) unreacted I2
Amount (mmoles) I2 reacted with C6H8O6

Amount (mmoles) C6H8O6 in Aliquot Portion

Total Amount (mmoles) C6H8O6 per tablet

C. Evaluation of the Drug


Mass (mg) C6H8O6 present / tablet
Average Mass (mg) of C6H8O6/tablet
Deviation
Standard Deviation
Coefficient of Variation (%RSD)

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Mass (mg) of C6H8O6/tablet Indicated on the Label

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Appendix A
Table 1. Some Important Acid-Base Indicators
(Arranged According to Increasing pH at which the Color Transition Occurs)

Color Transition Color of Acidic Color of Basic


Indicators
Range (pH) Species Species
Methyl violet 0.0-1.6 Yellow Violet
Cresol Red 0.2-1.8 Red Yellow
1.2-2.8 Red Yellow
Thymol Blue
8.0-9.6 Yellow Blue
Methyl Orange 3.1-4.4 Red Yellow
Congo Red 3.0-5.0 Violet Red
Bromocresol Green 3.8-5.4 Yellow Blue
Methyl Red 4.8-6.0 Red Yellow
Litmus 5.0-8.0 Red Blue
Bromothymol Blue 6.0-7.6 Yellow Blue
Phenol Red 6.8-8.4 Yellow Red
Cresol Purple 7.6-9.2 Yellow Purple
Phenolphthalein 8.3-10.0 Colorless Red
Alizarin Yellow 10.1-12.0 Yellow Orange-red

Appendix B

Table 2. Acid Dissociation Constants (Ka)

Acid Dissociation pKa


Weak Acid
Constants (Ka)
Acetic acid, CH3COOH 1.75 x 10-5 4.757
+ -10
Ammonium Ion, NH4 5.70 x 10 9.244
-5
Benzoic Acid, C6H5COOH 6.28 x 10 4.202
Formic acid, HCOOH 1.80 x 10-4 3.745
Methyl ammonium ion, CH3NH2 2.3 x 10-11 10.64
Phosphoric Acid, H3PO4 7.11 x 10-3 2.148
Dihydrogen phosphate, H2PO4- 6.32 x 10-8 7.199
Monohydrogen phosphate, HPO42- 4.5 x 10-13 12.35

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Work Sheets for Analytical Chemistry Lab1

Appendix C

Density of Water at 1 atmosphere


(from the Handbook of Chemistry and Physics, CRC press, 64th Ed.)

Temperature Density (g/cm3)


20 0.998207
21 0.997996
22 0.997774
23 0.997542
24 0.997300
25 0.9972994
26 0.9970480
27 0.9967870
28 0.9962371
29 0.9959486
30 0.9956511
31 0.9953450
32 0.9950302
33 0.9947070
34 0.9943756
35 0.9940359

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