LBYCH27 Worksheets
LBYCH27 Worksheets
LBYCH27 Worksheets
LBYCH27 WORKSHEETS
(ASA, D&C and Exercise
Sheets)
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.
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
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 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.
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
Experimental Procedure
A. Measurement of Mass
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.
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)
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)
Experiment 24
The Standardization of a Basic Solution and the
Determination of the Molar Mass of an Acid (Revised)
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.
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.
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.
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
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
a. Calculate the number of moles of HCl needed to reach the methyl orange end point.
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)
3. Draw the missing atoms to complete the structure of potassium hydrogen phthalate and encircle the acidic hydrogen.
4. How many moles of NaOH will react with the KHP dissolved in water?
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.
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:
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.
ID
Group No. Date
Number
Family Name
Given Name M.I.
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.
ID
Group No. Date
Number
Family Name
Given Name M.I.
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?
d. After adding the 25.00 mL solution of the weak acid and the 15.00 mL solution of the strong base together, the
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
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?
e. The pH of the solution when only the product sodium acetate is present in the solution.
C. Titration at Midpoint
Volume (mL) of DUS Titrated
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 _________________.
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
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 (pKa1) to (pKa1)
Before Mixing Before Mixing
(After Mixing)
CH3COOH NaCH3CO2
CH3COOH NaOH
HCl NaCH3CO2
NH4NO3 NH3
HNO3 NH3
NH4NO3 NaOH
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.
The ratio (mg Ca/mL) is the concentration of the EDTA solution expressed as Ca titer of EDTA.
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
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)
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
Table 1. Standardization of 0.02 M KMnO4 Against the Primary Standard Sodium Oxalate
Balanced Chemical Equation:
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.
_______________________________________________________________
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.
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-
8. Write the half reaction representing the transformation of OCl - (hypochlorite ion) to Cl-(chloride) in acidic medium.
9. Write the half reaction representing the transformation of l - (iodide ion) to I2 (iodine) in acidic medium.
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?
Titration Reaction:
Titration Reaction:
Titration Reaction:
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.
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
Back-Titration Reaction:
Appendix B
Appendix C