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EXPERIMENT 3
Purpose
To learn the technique to prepare an acid solution from a concentrated HCl and to
determine the accurate concentration of the HCl solution by standardization with standard
solution.
Introduction
Procedure
1. Read the label on the bottle of the concentrated HCl (should be located in the fume
hood). From the assay (% w/w, specific gravity and molecular weight) of the
concentrated HCl acid given, calculate the molarity of the concentrated HCl and
the volume needed to prepare 250 mL 0.1 M of dilute HCl solution.
2. Measure the calculated volume of the concentrated HCl (1) using a 10-mL
measuring cylinder and transfer into a 250 mL volumetric flask (which has already
contained some distilled water – to dilute conc. acid, add acid to water).
3. Rinse the measuring cylinder and transfer it into the volumetric flask. Then, dilute
the acid into the 250 mL of distilled water. Use a stopper to seal the volumetric
flask and mix well by turning the flask upside-down a few times in order for the
solution to be homogenous.
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1. Fill the burette with the prepared diluted HCl and record the initial burette reading.
2. Pipette 25.0 mL of the standard Na2CO3 that you have prepared in Exp. 2 into 250
mL conical flask. Add 2–3 drops of methyl orange as indicator.
3. Titrate the Na2CO3 in the conical flask with the HCl from the burette slowly while
shaking the flask until the indicator color changes from yellow to red. Record your
reading at the the end point of the titration.
4. Repeat 2–3 times and record all your readings in a table.
5. Calculate the exact molarity of your HCl solution.
6. Transfer the remaining acid solution into a clean reagent bottle
KEEP THIS SOLUTION FOR THE NEXT EXPERIMENT (i.e will be used
to standardize NaOH solution)
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ANALYTICAL CHEMISTRY
REPORT SHEET
Experiment No
Title
Name
Student ID
Course
Group
Date of Experiment
Date of Submission
Lecturer’s Name
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EXPERIMENT 3
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3. Results / Data
Obtain the following information from the label on the bottle of the concentrated HCl.
Table 1
Titration Rough 1 2 3
Final burette reading
Initial burette reading
Volume of HCl used
4. Questions
a) Based on the information in Table 2, calculate the molarity of the conc. HCl
solution.
b) What volume of the concentrated HCl is needed to prepare 250 mL 0.1 M HCl
solution?
c) Write a balanced equation for the reaction between HCl and Na2CO3.
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d) Using the data above and the stoichiometric ratio from the equation, calculate the
exact molarity of the HCl solution.
5. Conclusion
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EXPERIMENT 4
Purpose
Introduction
Vinegar is a diluted solution of acetic acid. Commercial vinegar should contain about 4-6
% of acetic acid (CH3COOH). The acetic acid content in vinegar can therefore be
determined through titration method using a standard solution of a base for example the
standard solution of NaOH. In this experiment, the acetic acid content in different brands of
commercial vinegar is to be determined by titrating them with NaOH solution that has
previously been standardized using a secondary standard solution of HCl (prepared in
Experiment 2).
Procedure
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1. Pipette 10 mL of the given vinegar (record the brand name of the chosen vinegar)
and dilute to mark with distilled water in a 100 mL volumetric flask.
2. Then pipette 20 mL of this diluted vinegar solution into a 250 mL conical flask.
Add 2 – 3 drops of phenolphthalein as an indicator.
3. Titrate the vinegar in the conical flask with the NaOH from the burette slowly
while shaking the flask until the indicator changes color.
4. Repeat steps 2 and 3 two more times.
5. Record your reading at the end point of the titration.
6. Calculate the w/v % of acetic acid in the vinegar sample.
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ANALYTICAL CHEMISTRY
REPORT SHEET
Experiment No
Title
Name
Student ID
Course
Group
Date of Experiment
Date of Submission
Lecturer’s Name
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EXPERIMENT 4
3. Results / Data
Titration Rough 1 2 3
Final burette reading
Initial burette reading
Volume of NaOH used
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Titration 1 2 3 4
Final burette reading
Initial burette reading
Volume of NaOH used
4. Questions
a) Write a balanced equation for the reaction between NaOH and HCl.
b) Using the data above and the stoichiometric ratio from the equation, calculate the
exact molarity of the NaOH solution.
c) Write the chemical equation for the reaction between acetic acid (CH3COOH) and
NaOH solution.
i) Using (MaVa / MbVb) = a/b, determine the molarity of the diluted acetic acid.
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ii) In the procedure 10 mL of the original vinegar has been diluted to 100 mL
Calculate the molarity of the concentrated (original) vinegar. (M1V1=M2V2)
iii) Calculate the mass of acetic acid (MW 60 g/mol) and then calculate % w/v
of acetic acid in the vinegar sample.
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g) Draw a titration curve for the titration between acetic acid (CH3COOH) and
NaOH solution.
5. Conclusion
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EXPERIMENT 5
Purpose
To determine the percent (w/w) of the active ingredient, acetlysalicyclic acid (C9H8O4) in
aspirin tablet.
Introduction
In this experiment the principle of back titration is being used to determine the excess mole
of NaOH and hence the mole of NaOH is consumed by acetylsalicylic acid in the reaction.
Calculations
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Procedure
A. Preparation of solution
Prepare 1 M NaOH solution (50 mL), 0.1 M HCl solution (250 mL) and 0.05 M
Na2CO3 (100 mL) as you have learned in previous experiments.
B. Hydrolysis of aspirin
1. Collect one commercial aspirin tablet (300 mg ASA) from your lecturer. Record the
brand name, the manufacturer’s name and % content (mass) of the active ingredient
in the tablet (use 2 tablets if the ASA content is 100 mg).
2. Weigh the aspirin tablet accurately in a weighing paper and transfer the tablets into
a 250 mL conical flask.
3. Add 25 mL (use pipette) 1.0 M NaOH solution and 25 mL of water to the tablet.
Heat this mixture until it boils for about 10 minutes in order to hydrolyze the
aspirin.
4. Cool the solution at room temperature then transfer quantitatively into 250 mL
volumetric flask. Dilute the solution to the mark carefully using dropper when the
level is close to the calibration mark.
D. Back titration
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ANALYTICAL CHEMISTRY
REPORT SHEET
Experiment No
Title
Name
Student ID
Course
Group
Date of Experiment
Date of Submission
Lecturer’s Name
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ANALYTICAL CHEMISTRY
EXPERIMENT 5
2. Describe the procedure (use schematic diagram if necessary). Show all the calculations
involved during the preparation of solutions.
A. Hydrolysis of aspirin
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3. Result/Data
Table 5.1
Name of manufacturer
Calculated % w/w
Titration Rough 1 2 3
Final burette reading
Initial burette reading
Volume of HCl used
Titration Rough 1 2 3
Final burette reading
Initial burette reading
Volume of HCl used
4. Calculation
a) Based on the data obtained in Table 5.2 calculate the exact molarity of HCl.
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b) Using back titration method, calculate the % (w/w) aspirin in the aspirin tablet.
ii) Based on Equation (2), calculate the mole of excess (unreacted) NaOH.
iii) Calculate the mole of NaOH that has actually reacted with acetylsalicylic acid.
iv) Based on Equation (1), calculate the mole of acetylsalicylic acid in the
solution.
v) Calculate the mass then the % w/w of acetylsalicylic acid in the tablet.
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vi) Compare the % w/w calculated in Table 5.1 and the result obtained in (e).
Calculate the % error.
5. Conclusion
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EXPERIMENT 12
GRAVIMETRY II: GRAVIMETRIC ANALYSIS OF PHOSPHORUS
IN PLANT FOOD
Purpose
Introduction
Gravimetric analysis is a quantitative method that is based on determining the mass of pure
compound to which the analyte is chemically related. In the method, the analyte is
selectively converted to an insoluble precipitate; the precipitate is then dried or ignited and
accurately weighed. Gravimetric analysis is considered as one of the most accurate method
of chemical analysis. Usually, gravimetric analyses involve the following steps:
Plant foods contain three essential nutrients; nitrogen, phosphorus and potassium. The
labels on the plant food usually have a set of numbers such as 15-30-15 which indicate the
content % of the nutrient (15% N, 30% P (expressed as P2O5) and 15% K (expressed as
K2O). The remainder is either anions or cations necessary to balance the charge in the
chemical compounds.
5H2O (l) + HPO42- (aq) + NH4 + (aq) + Mg2+ (aq) + OH- (aq) MgNH4PO4.6H2O (s)
The % P and % P2O5 in the initial sample can be calculated from the mass of
MgNH4PO46H2O obtained using the following method:
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Procedure
1. Obtain your plant food sample and record the set of numbers written on the label.
2. Weigh the plant food sample between 3.0 - 3.5 g using a weighing paper and transfer
the sample to a 250 mL beaker.
3. Add 35 - 40 mL of distilled water and stir the mixture with a glass rod to dissolve the
sample. If your sample does not completely dissolve, remove the insoluble material
through filtration.
4. To filtrate, add about 40 mL of 10% MgSO4.7H2O. Then add about 100 mL 2 M NH3
(aq) slowly while stirring. A white precipitate of MgNH4PO4.6H2O will form.
5. Allow the mixture to sit at room temperature for 10 minutes to complete the
precipitation.
6. Weigh accurately a filter paper. Fold the paper and fit it into a glass funnel. Wet the
paper with distilled water to hold it in place in the funnel. Transfer the precipitate
carefully and all the solution from the beaker onto the filter paper.
7. Wash the precipitate by adding 2 - 3 times of 5 mL portions of distilled water to the
beaker. Then rinse again the precipitate with two 10 mL portions of 75% isopropyl
alcohol through the filter paper.
8. Remove the filter paper, place it on a numbered porcelain evaporating dish and store it
to dry for 2 - 3 days on the bench or dry in the oven for 24 hrs at 60oC.
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9. When the MgNH4PO4.6H2O is thoroughly dry, weigh the filter paper plus the
MgNH4PO4.6H2O. Record the mass and calculate the % of phosphorus in your original
sample.
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ANALYTICAL CHEMISTRY
REPORT SHEET
Experiment No
Title
Name
Student ID
Course
Group
Date of Experiment
Date of Submission
Lecturer’s Name
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EXPERIMENT 12
3. Results / Data
4. Calculation
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c) Compare your result from the amount (w/w %) stated on the label of the plant food.
Calculate the % error.
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5. Conclusion
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