Laboratory Manual Qc1 1
Laboratory Manual Qc1 1
Laboratory Manual Qc1 1
Activity No. 1
Common Apparatus used in Pharmaceutical Analysis
Objectives:
1. To review on the different apparatus commonly used in drug
assaying and quality control.
2. To familiarize the uses and basic care for each apparatus.
3.
4.
Materials:
buret wash bottle
pipette reagent bottle
volumetric flask watch glass
crucible and cover stirring rod
evaporating dish Fischer stand
aspirator water bath
pH meter iodine flask
funnel suction flask
graduated cylinder cassia flask
spatula separatory funnel
water bath beaker
Procedure:
1. Wash the apparatus given by the instructor.
2. Complete the table given below.
1
2.
3.
4.
5.
6.
7.
2
8.
9.
10.
11.
12.
13.
3
14.
15.
16.
17.
18.
19.
4
20.
21.
22.
Questions:
1. What is the use of cleaning solution? Enumerate the different cleaning
solutions for glasswares.
5
3. Differentiate accuracy from precision.
Conclusion:
6
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 2
General Operations and Common Methods in
Pharmaceutical Analysis
Objectives:
1. To familiarize the methods commonly used in pharmaceutical
analysis.
2. To identify the proper use and care of an analytical balance.
3.
4.
Materials:
analytical balance pipet
watch glass aspirator
any tablets or capsules beaker
forceps dropper
stirring rod
Procedure:
A. The Analytical Balance
1. Use the balance assigned by the instructor.
2. Make sure that the balance bubble located at the bottom is at the
center.
3. The balance pan must be empty and clean, and the doors must be all
closed.
4. Weigh the sample given carefully. Record.
5. Calculate the mean, range, average deviation, relative average
deviation, standard deviation and relative standard deviation.
B. Pipetting
1. Clean the pipet thoroughly before each use. Wash it first with the
liquid to be measured. Discard the washings.
2. Measure the amount of liquid designated by the instructor.
3. Use the aspirator in filling the pipet. DO NOT USE YOUR MOUTH!
4. Fill the pipet and drain the liquid down to the desired mark. DO NOT
DRAIN THE PIPET BY BLOWING!
5. Read the lower meniscus when measuring colorless liquid and upper
meniscus if it is a highly colored liquid.
6. Follow the proper way of pipetting as illustrated below.
7
C. The Use of Indicators
1. Prepare six beakers. Fill the first three beakers with 10 mL 0.1 N acid
and the other three beakers with 10 mL 0.1 N alkali solution.
2. Add 2-3 drops of indicators (methyl red, methyl orange,
phenolphthalein) to each beaker of acid and alkali.
3. Observe the resulting colors.
4. Add 2 mL of alkali solution to the beakers with diluted acid and 2 mL
diluted acid to the beakers with alkali solution. Observe.
5. Then, add an additional 8 mL of alkali solution to the beakers with
diluted acid and 8 mL diluted acid to the beakers with alkali solution.
Observe the resulting color.
8
*Show your solution below. Encircle the mean, absolute error, relative
error, range, average deviation, relative average deviation, standard
deviation and relative standard deviation.
9
Questions:
1. Why should an analytical balance be used in analytical assay? Draw
and label the parts of an analytical balance.
2. What is the reason why the doors of the balance must be closed before
reading the weight?
Conclusion:
10
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 3
Preparation and Standardization of 0.1 N Hydrochloric
Acid
Objectives:
1. To prepare and standardize 0.1N hydrochloric acid.
2. To appreciate the importance of standardizing solutions of
known concentration.
3.
4.
Chemicals Needed:
Hydrochloric Acid (HCl)
Sodium Carbonate (Na2CO3)
Methyl Red T.S.
Procedure:
A. Preparation
1. Dilute 4.2 mL of conc. HCl to 500 mL with water.
2. Allow to cool to room temperature.
B. Standardization
1. Weigh accurately about 0.1 – 0.15 g of primary standard anhydrous
Na2CO3 that previously has been heated at a temperature of about 270°C
for 1 hour.
2. Dissolve it in 100 mL of water, and add 2 drops of methyl red T.S.
3. Add the acid slowly from the buret with constant stirring, until the
solution becomes faintly pink.
4. Heat the solution to boiling and continue the titration.
5. Heat again to boiling, and titrate further as necessary until the end
point is no longer affected by the continued boiling.
6. Calculate the normality.
11
Data Trial 1 Trial 2
Weight of Na2CO3 (g)
Volume of HCl consumed (mL)
Normality
Average Normality
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
12
3. What is primary standard? secondary standard? Give at least three
examples each.
Conclusion:
13
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 4
Preparation and Standardization of 0.1 N Sodium
Hydroxide
Objectives:
1. To prepare and standardize 0.1 N sodium hydroxide solution.
2. To appreciate the importance of standardizing solutions of
known concentration.
3.
4.
Chemicals Needed:
Sodium Hydroxide (NaOH) pellets
Potassium Biphthalate (KHC8H4O4)
Phenolphthalein T.S.
Procedure:
A. Preparation
1. Dissolve 5.2 g of NaOH pellets in 300 mL water.
2. Cool the solution and filter to a 500-mL volumetric flask.
3. Add sufficient quantity of water to volume.
4. Transfer the solution to your container and add another 500 mL of
water.
B. Standardization
1. Weigh accurately about 0.3-0.4 g of KBP, previously crushed lightly
and dried at 120°C for 2 hours.
2. Dissolve it in 75 mL of water.
3. Add 2 drops of phenolphthalein T.S.
4. Titrate with the NaOH solution until it produces a permanent pink
color.
5. Calculate the normality.
14
Data and Results:
A. Data Obtained
Titer value of KBP: ________
Data Trial 1 Trial 2
Weight of KBP (g)
Volume of NaOH consumed (mL)
Normality
Average Normality
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
15
3. Discuss how an alkali solution should be stored.
Conclusion:
16
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 5
Preparation and Standardization of 0.1 N Sulfuric Acid
Objectives:
1. To prepare and standardize 0.1 N Sulfuric Acid solution.
2. To determine the importance of standardizing solutions.
3.
4.
Chemicals Needed:
Sulfuric Acid (H2SO4)
0.1 N NaOH VS
Phenolphthalein T.S.
Procedure:
A. Preparation
1. Using a pipet, add slowly 1.5 mL of conc. H2SO4 to about 400 mL of
distilled water in a 500-mL volumetric flask, while stirring continuously.
2. Add enough water to volume.
B. Standardization
1. In to an Erlenmeyer flask, transfer using a buret or pipet 15 mL of
H2SO4 to be standardized.
2. Add 2 drops of phenolphthalein T.S. slowly.
3. Add from a buret the previously standardized NaOH until a light pink
color is obtained, while swirling constantly.
4. Compute the normality.
17
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
18
5. If 20 mL of a NaOH solution required 24.8 mL of a H2SO4 solution in a
titration and 25 mL of the acid solution was required in the titration of
0.3062 g pure Na2CO3, what was the normality of the NaOH solution?
Conclusion:
19
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 6
Assay of Sodium Bicarbonate
Objectives:
1. To assay sodium bicarbonate by direct acidimetric analysis.
2.
3.
Chemicals Needed:
Sodium Bicarbonate (NaHCO3)
0.1 N H2SO4 VS
Methyl Orange T.S.
Procedure:
1. Weigh accurately 0.2-0.3 g of NaHCO3.
2. Mix with 25 mL of water.
3. Add 2-3 drops of methyl orange T.S.
4. Titrate with 0.1 N H2SO4 VS.
5. Calculate the % purity of NaHCO3.
B. Calculations:
(label properly)
20
C. Chemical Reaction Involved:
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion:
21
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 7
Assay of Milk of Magnesia
Objectives:
1. To assay the magnesium hydroxide content of milk of magnesia
by residual acidimetric analysis.
2. To differentiate direct titration from residual titration.
3.
4.
Chemicals Needed:
Milk of Magnesia
0.1 N NaOH
0.1 N H2SO4
Methyl Red T.S.
Procedure:
1. Weigh 0.5-0.7 g of milk of magnesia in an Erlenmeyer flask.
2. Add 25 mL of 0.1 N H2SO4 using a buret.
3. Add 3 drops of methyl red T.S.
4. Titrate the excess with 0.1 N NaOH until a yellow color is produced.
22
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
23
4. Give at least 10 substances assayed under residual acidimetry.
Conclusion:
24
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 8
Assay of Tartaric Acid
Objectives:
1. To assay tartaric acid by direct alkalimetric analysis.
2. To differentiate acidimetric and alkalimetric analysis.
3.
4.
Chemicals Needed:
Tartaric Acid (H2C4H4O6)
0.1 N NaOH VS
Phenolphthalein T.S.
Procedure:
1. Place about 0.35 g of H2C4H4O6 accurately weighed in an Erlenmeyer
flask.
2. Dissolve it in 40 mL distilled water.
3. Add 2 drops of phenolphlthalein T.S.
4. Titrate with 0.1 N NaOH VS until a permanent pink color is obtained.
B. Calculations:
(label properly)
25
C. Chemical Reaction Involved:
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion:
26
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 9
Assay of Aspirin Tablets
Objectives:
1. To assay aspirin (ASA) tablets by residual alkalimetric titration.
2. To determine how neutralized alcohol is prepared.
3.
4.
Chemicals Needed:
ASA tablets 0.1 N NaOH
0.1 N H2SO4 95% Alcohol
Phenolphthalein T.S.
Procedure:
1. Weigh and finely powder not less than 10 tablets.
2. Transfer an accurately weighed amount of the powdered tablets
equivalent to 100 mg of ASA in a 250 mL Erlenmeyer flask.
3. Add 15 mL of *neutralized alcohol and mix for 5 minutes.
4. Then add 3 drops of phenolphthalein T.S. and titrate with 0.1 N NaOH
until pink color is produced.
5. Add to the titrated solution a volume of 0.1 NaOH equal to that used
in the titration plus 15 mL excess.
6. Heat the mixture in a water bath for 15 minutes. Swirl the flask
occasionally.
7. Remove the flask from the water bath and cool quickly to room
temperature.
8. Titrate with 0.1 N H2SO4 until the pink color disappears.
9. Perform a blank titration.
27
Data Result (Sx) Result (Bl)
Weigh of ASA (mg)
N of NaOH
Volume of NaOH used (mL)
N of H2SO4
Volume of H2SO4 used (mL)
Difference of the 2 volumes (H2SO4)
Content of ASA
% Labeled amount
B. Calculations:
(label properly)
𝐴𝑆𝐴 (𝑉𝑏𝑙 − 𝑉𝑠𝑥)𝑥 𝑁 𝑎𝑐𝑖𝑑 𝑥 𝑚𝑒𝑞 𝑤𝑡 𝑜𝑓 𝐴𝑆𝐴
𝐶𝑜𝑛𝑡𝑒𝑛𝑡 𝑜𝑓 .= 𝑥 𝐴𝑣𝑒. 𝑤𝑒𝑖𝑔ℎ𝑡
𝑡𝑎𝑏 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
28
2. What is the reason of adding neutralized alcohol in the assay?
Conclusion:
29
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 10
Preparation and Standardization of 0.1 N Silver Nitrate
Objectives:
1. To prepare and standardize 0.1 N silver nitrate solution for use
in the succeeding volumetric precipitation exercises.
2. To define precipitimetry.
3.
4.
Chemicals Needed:
Silver Nitrate (AgNO3) crystals
Sodium Chloride (NaCl) reagent grade
Acetic Acid (CH3COOH)
Methanol
Eosin Y T.S.
Procedure:
A. Preparation
1. Weigh accurately 4.375 g AgNO3 crystals.
2. Dissolve in a sufficient amount of water.
3. Transfer to a 250-mL volumetric flask.
4. Add sufficient amount of water to volume. Mix thoroughly.
B. Standardization
1. Transfer about 100 mg accurately weighed NaCl (reagent grade),
previously dried at 110°C for 2 hours, to an erlenmeyer flask.
2. Dissolve in 5mL water and add 5 mL of CH3COOH, 50 mL methanol.
3. Add about 0.5 mL Eosin Y T.S.
4. Stir preferably with magnetic stirrer.
5. Titrate with AgNO3 solution until greenish-yellow color is produced.
30
Data Trial 1 Trial 2
Weight of NaCl (g)
Volume of AgNO3 consumed (mL)
Normality
Average Normality
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
31
4. Is there other way of standardizing AgNO3? If yes, how it is done?
Conclusion:
32
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 11
Preparation and Standardization of 0.1 N Ammonium
Thiocyanate
Objectives:
1. To prepare and standardize 0.1 N ammonium thiocyanate for
use in the succeeding precipitation exercises.
2. To enumerate the different chemical indicators used in
precipitation method of analysis.
3.
4.
Chemicals Needed:
Ammonium Thiocyanate (NH4SCN), reagent grade
0.1 N AgNO3 VS
Ferric Ammonium Sulfate (NH4Fe(SO4)2) T.S.
Nitric Acid (HNO3)
Procedure:
A. Preparation
1. Dissolve about 2 g (plus 0.2 g excess) of NH4SCN (reagent grade) in
enough water to make 250-mL.
B. Standardization
1. Place 15 mL of 0.1 N AgNO3 accurately measured from a buret in an
erlenmeyer flask.
2. Dilute with 25 mL of distilled water, then add 1 mL HNO3.
3. Add 1 mL NH4Fe(SO4)2 T.S.
4. Titrate the solution with the NH4SCN solution until a red-brown color
appears.
33
Average Normality
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion
34
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 12
Assay of Sodium Lauryl Sulfate for Sodium Chloride
Content
Objectives:
1. To assay sodium lauryl sulfate for NaCl content by direct
precipitimetric method.
2. To identify other substances assayed under such method.
3.
4.
Chemicals Needed:
Sodium Lauryl Sulfate (SLS)
HNO3
0.1 N AgNO3 VS
Potassium Chromate (K2CrO4) T.S.
Procedure:
1. Dissolve about 2 g SLS, accurately weighed, in about 20 mL of water.
2. Neutralize the solution with diluted HNO3 (1:20), using litmus paper
as the indicator.
3. Add 2 mL of K2CrO4 T.S.
4. Titrate with 0.1 N AgNO3 until there is a formation of red precipitates.
35
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion:
36
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 13
Assay of Sodium Chloride
Objectives:
1. To assay sodium chloride by residual precipitimetry (Volhard
method).
2. To identify other substances assayed under the process
mentioned above.
3.
4.
Chemicals Needed:
any NaCl available in the market
HNO3
Nitrobenzene (C6H5NO2)
0.1 N AgNO3 VS
0.1 N NH4SCN VS
NH4Fe(SO4)2 T.S.
Procedure:
1. Weigh accurately about 250 mg NaCl.
2. Dissolve it in 50 mL distilled water in a glass-stoppered flask.
3. Add 50 mL of 0.1 N AgNO3 VS, 3 mL of HNO3, 5 mL C6H5NO2, and 2
mL NH4Fe(SO4)2 T.S.
4. Shake well, and titrate the excess AgNO3 with 0.1 N NH4SCN VS until
the appearance of red brown color.
37
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion:
38
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 14
Preparation and Standardization of 0.05 M Disodium EDTA
Objectives:
1. To prepare and standardize 0.05 M Disodium
Ethylenediaminetetraacetic Acid (EDTA) solution for use in complexation
method of analysis.
2. To determine the properties and characteristics of Na2EDTA.
3.
4.
Chemicals Needed:
Na2EDTA
Calcium Carbonate (CaCO3)
Diluted HCl
NaOH T.S.
Hydroxynaphthol blue
Procedure:
A. Preparation
1. Dissolve about 4.7 g of Na2EDTA powder in sufficient distilled water to
make 250 mL of solution.
B. Standardization
1. Weigh accurately about 200 mg of CaCO3 (previously dried at about
110°C for about 2 hours).
2. Transfer to a cleaned and dried flask and add about 10 mL of water
with gentle stirring to form slurry.
3. Cover with a watch glass and introduce 2 mL diluted HCl.
4. Swirl the contents until dissolve.
5. Add 100 mL distilled water to the solution washing the sides of the
beaker, pipet and watch glass.
6. While stirring the solution, preferably with a magnetic stirrer, add
about 30 mL of Na2EDTA solution from a buret.
7. Add 15 mL of NaOH T.S. with constant stirring.
8. Add 300 mg of hydroxynaphthol blue indicator.
9. Continue the titration with the Na2EDTA solution to a blue endpoint.
39
*This exercise will serve both the standardization and the assay of
calcium.
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
40
2. Why is disodium EDTA was used instead of free EDTA in preparing the
standard solution?
Conclusion:
41
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 15
Preparation and Standardization of 0.1 N Potassium
Permanganate
Objectives:
1. To prepare and standardize 0.1 N potassium permanganate to
use in the succeeding assay involving oxidation-reduction method of
analysis.
2.
3.
Chemicals Needed:
Potassium Permanganate (KMnO4)
Sodium Oxalate (Na2C2O4)
Procedure:
A. Preparation
1. Dissolve about 0.825 g of KMnO4 crystals in enough water to make
250 mL solution in a flask.
2. Boil the solution for about 15 minutes.
3. Stopper the flask and allow it to stand for at least 2 days.
4. Filter through asbestos.
B. Standardization
1. Weigh accurately about 200 mg of Na2C2O4, previously dried at 110°C
to constant weight.
2. Dissolve it in 250 mL water.
3. Add 7 mL of H2SO4, heat to about 70°C.
4. Titrate immediately the heated solution with the KMnO4 from the
buret. Swirl the contents constantly while titrating, until a pale pink
color which persists for 15 seconds is produced.
5. The temperature at the conclusion of the titration should not be less
than 60°C.
42
Volume of KMnO4 consumed (mL)
Normality
Average Normality
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
2. What is the reason for boiling the KMnO4 for about 15 minutes and
allowing it to stand for at least 2 days?
43
3. Give the rationale why the solution was filtered through asbestos.
Conclusion:
44
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 16
Assay of Hydrogen Peroxide Solution
Objectives:
1. To assay hydrogen peroxide by permanganate method of
analysis under oxidation-reduction process.
2. To define the process of oxidation and reduction.
3.
4.
Chemicals Needed:
3% Hydrogen Peroxide (H2O2)
Diluted H2SO4
0.1 N KMnO4 VS
Procedure:
1. Pipet 2 mL H2O2 into a suitable flask containing 20 mL water.
2. Add 20 mL diluted H2SO4.
3. Titrate with 0.1 N KMnO4 VS until a permanent pink color is
produced.
45
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
3. What is the reason for conducting the titration for H2O2 in an acid
solution?
46
4. State two properties or characteristics of H2O2 topical solution?
Conclusion:
47
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 17
Preparation and Standardization of 0.1 N Iodine Solution
Objectives:
1. To prepare and standardize 0.1 N iodine solution for use in the
oxidation-reduction methods of analysis – iodimetry and iodometry.
2.
3.
Chemicals Needed:
Iodine (I2) NaHCO3
Potassium Iodide (KI) Starch T.S.
Arsenic Trioxide (As2O3) Methyl Orange solution
1 N NaOH
Diluted HCl
Procedure:
A. Preparatiom
1. Dissolve about 3.5 g of I2 in a solution of 9 g of KI in 30 mL of water.
2. Add 3 drops of diluted HCl.
3. Add sufficient amount of water to make 250 mL.
B. Standardization
1. Weigh accurately about 100-150 mg of As2O3, previously dried at
105°C for 1 hour. Transfer to a 500-mL erlenmeyer flask.
2. Dissolve in 20 mL of 1 N NaOH. Warm the solution of necessary.
3. Dilute with 40 mL water.
4. Add 2 drops of methyl orange solution.
5. Add diluted HCl drop by drop until the solution turns yellow to pink.
6. Add 2 g of NaHCO3.
7. Dilute with 50 mL water.
8. Add 3 mL starch T.S.
9. Titrate with I2 solution from a buret until a permanent blue color
solution is produced.
48
Data Trial 1 Trial 2
Weight of As2O3 (g)
Volume of I2 sol. consumed (mL)
Normality
Average Normality
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
49
3. Why does iodine produce a blue reaction with starch T.S.?
Conclusion:
50
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 18
Assay of Ascorbic Acid
Objectives:
1. To assay ascorbic acid by iodimetric method under oxidation-
reduction process.
2. To list down standard solutions classified as reducing and
oxidizing agent.
3.
4.
Chemicals Needed:
Ascorbic Acid (C6H8O6)
2 N H2SO4
Starch T.S.
Procedure:
1. Dissolve about 300 mg ascorbic acid in a mixture of 100 mL of water
and 20 mL of 20 N H2SO4.
2. Add 3 mL of starch T.S.
3. Titrate with 0.1 N I2 solution until blue color appears.
51
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
52
4. Give the synonym of ascorbic acid and its uses.
Conclusion:
53
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 19
Preparation and Standardization of 0.1 N Sodium
Thiosulfate
Objectives:
1. To prepare and standardize 0.1 N sodium thiosulfate to be used
for analysis by oxidation-reduction (iodimetric and iodometric) methods.
2. To list down standard solutions used in iodimetric and
iodometric methods.
3.
4.
Chemicals Needed:
Sodium Thiosulfate (Na2S2O3) Potassium Dichromate (K2Cr2O7)
Na2CO3 KI
NaHCO3 HCl
Starch T.S.
Procedure:
A. Preparation
1. Boil and cool water about 300 mL.
2. Dissolve about 6.25 g Na2S2O3 and 50 mg of Na2CO3 in a sufficient
amount of recently boiled and cooled water.
3. Transfer to a 250-mL volumetric flask and dilute to volume.
B. Standardization
1. Weigh accurately about 100-150 mg of primary standard K2Cr2O7
(previously pulverized and dried at 120°C for 4 hours).
2. Dissolve in 100 mL of water in a glass-stoppered flask.
3. Swirl to dissolve the sample.
4. Remove the stopper, and quickly add 3 g of KI, 2 g NaHCO3 and 5 mL
HCl.
5. Stopper the flask. Swirl to mix.
6. Allow to stand in dark for 10 minutes.
7. Rinse the stopper and the inner walls of the flask with water.
8. Titrate the liberated iodine with the Na2S2O3 until the solution is only
faintly yellow in color.
9. Add 3 mL starch T.S.
10. Continue the titration to the discharge of the blue color.
54
Data and Results:
A. Data Obtained
Titer value of K2Cr2O7: ________
Data Trial 1 Trial 2
Weight of K2Cr2O7 (g)
Volume of Na2S2O3 consumed (mL)
Normality
Average Normality
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
2. The water used to dissolve Na2S2O3 was boiled and cooled. Why?
55
3. What are the other ways to standardize Na2S2O3?
Conclusion:
56
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 20
Assay of Sodium Hypochlorite Solution
Objectives:
1. To assay the sodium hypochlorite content of the commercially
available brands by oxidation-reduction, iodometric method.
2. To differentiate iodimetry and iodometry.
3.
4.
Chemicals Needed:
Sodium Hypochlorite solution (any brand) (NaClO)
KI
CH3COOH
0.1 N Na2S2O3 VS
Starch T.S.
Procedure:
1. Weigh accurately about 3 mL NaClO solution.
2. Dilute it with 50 mL water.
3. Add 2 g of KI.
4. Add 10 mL CH3COOH.
5. Titrate the liberated I2 with 0.1 N Na2S2O3 until yellowish brown.
6. Immediately add 3 mL starch T.S. and continue the titration until the
blue color disappears.
57
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
58
4. How iodine was liberated in the experiment?
Conclusion:
59
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 21
Assay of Sodium Lauryl Sulfate for Sodium Sulfate
Content
Objectives:
1. To assay the sodium sulfate content of sodium lauryl sulfate by
gravimetric analysis.
2. To define gravimetric analysis.
3.
4.
Chemicals Needed:
Sodium Lauryl Sulfate (SLS)
Alcohol
HCl
Barium Chloride T.S.(BaCl2)
Procedure:
1. Transfer about 1 g of SLS, accurately weighed, to a 500-mL beaker.
2. Add 10 mL of water.
3. Heat the mixture, and stir until completely dissolved.
4. To the hot solution, add 100 mL alcohol.
5. Cover the beaker.
6. Digest at a temperature just below the boiling point for 2 hours.
7. Filter, while hot, through a filtering crucible.
8. Wash the precipitate with 100 mL of hot water, collecting the washings
in a beaker.
9. Acidify with 10 mL of HCl. Heat to boiling.
10. Add 25 mL of BaCl2 T.S. allow to stand overnight.
11. Collect the precipitate in a tared filtering crucible.
12. Wash until free from chloride, dry, ignite, and weigh.
*In the use of ashless filter paper, dry first the crucible to be used at
120°C until constant in weight.
60
Data Results
Weight of the SLS (g)
Volume of alcohol used (mL)
Volume of HCl (mL)
Weight of BaSO4 (product)
% Na2SO4
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
61
4. What is the purpose of heating the precipitate mixture of BaSO4 for an
hour over a water bath?
Conclusion:
62
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 22
Water Content Determination
Objectives:
1. To determine the water content of available powder from a plant
material in the laboratory.
2. To determine the importance of water content determination of
crude drugs.
3.
4.
Chemicals Needed:
Acacia Tragacanth
Veegum
Procedure:
1. Sieve the sample powder to achieve uniform particle size.
2. Weigh a clean, dried and empty crucible. Without removing the
crucible, add a sufficient amount of the sample powder. Record the
weights obtained.
3. Dry at 105°C for 5 hours, and weigh.
4. Continue the drying and weighing at 1-hr interval until the loss in not
more than 0.25% in 1 hour of drying.
B. Calculations:
(label properly)
𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 = 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑝𝑜𝑤𝑑𝑒𝑟 − 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑑𝑟𝑖𝑒𝑑 𝑝𝑜𝑤𝑑𝑒𝑟
63
𝑚𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝑐𝑜𝑛𝑡𝑒𝑛𝑡
% 𝑚𝑜𝑖𝑠𝑡𝑢𝑟𝑒 = 𝑥 100
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑝𝑜𝑤𝑑𝑒𝑟
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion:
64
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 23
Assay of Aloe
Objectives:
1. To determine the water-soluble extractive of aloe.
2. To define extractive.
3.
4.
Chemicals Needed:
Aloe-containing products
Distilled water
Procedure:
1. Macerate about 2 g of the prepared, accurately weighed, in about 70
mL of distilled water in a suitable flask.
2. Shake the mixture during 8 hours at 30-min intervals.
3. Allow the mixture to stand for 16 hours without shaking.
4. Filter and wash the flask and residue with small portions of distilled
water, passing the washings through the filter, until the filtrate measures
100 mL.
5. Weigh the residue.
6. Evaporate a 50-mL aliquot portion of this filtrate to dryness.
7. Dry to constant weight at 110°C.
65
B. Calculations:
(label properly)
Questions:
1. Define extractive. Why is it used as an index of purity?
Conclusion:
66
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 24
Acid Value Determination of Olive Oil
Objectives:
1. To determine the acid value of olive oil.
2. To define acid value.
3.
4.
Chemicals Needed:
Olive oil 0.1 N NaOH
95% Alcohol Phenolphthalein T.S.
Procedure:
1. Weigh 10 g of the oil in a flask.
2. Neutralize 15 mL of alcohol with 0.1 N NaOH as the titrant and
phenolphthalein T.S. as the indicator.
3. Add this neutralized alcohol to the oil in the flask.
4. Mix thoroughly.
5. Add 3 drops of phenolphthalein T.S.
6. Titrate the solution with 0.1 N NaOH until the solution becomes faintly
pink after being shaken for 30 seconds.
67
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
2. Define the term acid value. What is the implication of a high acid
value?
3. Why must the alcohol used as solvent for oil in acid value
determination be neutral?
68
4. What is/are the cause/s of the presence of free acids in oils?
5. Find the acid number of almond oil weighing 0.7 g which required
17.9 mL of 0.1017 N NaOH to bring about the end point.
Conclusion:
69
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 25
Preparation and Standardization of 0.5 N Hydrochloric
Acid
Objectives:
1. To prepare and standardize 0.5 N HCl solution.
2.
3.
Chemicals Needed:
Conc. HCl Na2CO3
Methyl Red T.S.
Procedure:
A. Preparation
1. Dilute 12 mL of HCl in water to make 250 mL.
B. Standardization
1. Weigh accurately 0.6 g of Na2CO3 that has been previously heated at
270°C for 1 hour.
2. Dissolve it in 100 mL of water.
3. Add 2 drops of methyl red T.S.
4. Titrate with 0.5 N HCl until faintly pink.
5. Heat the solution to boiling, and continue the titration until the pale
pink color is no longer affected by the continuous boiling.
70
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion:
71
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 26
Saponification Value of Cooking Oil
Objectives:
1. To determine the saponification value of any brand of cooking oil
available in the market.
2. To define saponification value.
3.
4.
Chemicals Needed:
Cooking oil, any brand 0.5 N HCl VS
0.5 N Alcoholic Potassium Hydroxide (KOH)
Phenolphthalein T.S.
Procedure:
1. Place 1.0-1.5 g of the oil sample, accurately weighed in an erlenmeyer
flask.
2. Add 20 mL from a buret alcoholic 0.5 N KOH solution.
3. Heat the flask on a water bath for 30 minutes, frequently rotating the
contents.
4. Add 1 mL phenolphthalein T.S.
5. Titrate the excess of KOH with 0.5 N HCl until the pink color
disappears.
6. Perform a blank determination.
72
B. Calculations:
(label properly)
𝑚𝑔
(𝑉𝑏𝑙 − 𝑉𝑠𝑥)𝑥 𝑁 𝐻𝐶𝑙 𝑥
𝑚𝑒𝑞 𝑜𝑓 𝐾𝑂𝐻
𝑆𝑉 =
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑡ℎ𝑒 𝑠𝑎𝑚𝑝𝑙𝑒
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
73
4. If a sample of beeswax has an acid value of 1.7 and a saponification
value of 187.3, what is the ester value of the sample? Does it conforms to
standard?
Conclusion:
74
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Exercise No. 27
Assay of Phenol Content of Clove Oil
Objectives:
1. To determine the phenol (eugenol) content of clove oil using
cassia flask.
2. To be able to use the cassia flask properly.
3.
4.
Chemicals Needed:
Clove Oil
KOH T.S.
Procedure:
1. Pipet 10 mL of clove oil into a cassia flask. Add 75 mL of KOH T.S.
2. Shake the mixture for 5 minutes, and heat for 10 minutes in boiling
water. Shake the flask at least three times during the heating.
3. Remove the flask from the bath, and cool to room temperature.
4. When the liquids have separated completely, add sufficient KOH T.S.
to raise the lower limit of the oily layer within the graduated portion of
the neck.
5. Read the volume of the oil.
75
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion:
76
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 28
Preparation and Standardization of 0.02 N Sodium
Hydroxide
Objectives:
1. To prepare and standardize 0.02 N sodium hydroxide solution
for use in the assay of alkaloid content in coffee powder.
2.
3.
Chemicals Needed:
Sodium Hydroxide (NaOH) pellets
Potassium Biphthalate (KHC8H4O4)
Phenolphthalein T.S.
Procedure:
A. Preparation
1. Dissolve 0.25 g of NaOH pellets in 150 mL water.
2. Cool the solution and filter to a 250-mL volumetric flask.
3. Add sufficient quantity of water to volume.
B. Standardization
1. Weigh accurately about 0.1-0.2 g of KBP, previously crushed lightly
and dried at 120°C for 2 hours.
2. Dissolve it in 75 mL of water.
3. Add 2 drops of phenolphthalein T.S.
4. Titrate with the NaOH solution until it produces a permanent pink
color.
5. Calculate the normality.
77
Data Trial 1 Trial 2
Weight of KBP (g)
Volume of NaOH consumed (mL)
Normality
Average Normality
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion:
78
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 29
Preparation and Standardization of 0.02 N Sulfuric Acid
Objectives:
1. To prepare and standardize 0.02 N Sulfuric Acid solution for use
in the assay of alkaloidal content of coffee powder.
2.
3.
Chemicals Needed:
Sulfuric Acid (H2SO4)
0.1 N NaOH VS
Phenolphthalein T.S.
Procedure:
A. Preparation
1. Using a pipet, add slowly 0.15 mL of conc. H2SO4 to about 200 mL of
distilled water in a 250-mL volumetric flask, while stirring continuously.
2. Add enough water to volume.
B. Standardization
1. In to an Erlenmeyer flask, transfer using a buret or pipet 15 mL of
H2SO4 to be standardized.
2. Add 2 drops of phenolphthalein T.S. slowly.
3. Add from a buret the previously standardized NaOH until a light pink
color is obtained, while swirling constantly.
4. Compute the normality.
79
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
Conclusion:
80
Name: _______________________________ Date: _____________
Group Number: _________ Score: _________
Activity No. 30
Assay of Caffeine Alkaloid in a Coffee Powder
Objectives:
1. To determine the caffeine content of coffee powders available in
the market.
2. To differentiate proximate and ultimate assay.
3.
4.
Chemicals Needed:
Coffee powder Chloroform
0.02 N NaOH VS Methyl Red T.S.
0.02 N H2SO4 VS Distilled water
1 N NaOH
Procedure:
1. Weigh 1 g of coffee powder and dissolve in 50 mL hot water.
2. Add 8 mL of 1 N NaOH, cool the solution.
3. Transfer the solution in a separatory funnel. Shake gently.
4. Add three successive portions, one at a time, 15 mL each of
chloroform. For every extraction, shake the funnel for about 5 minutes.
5. Filter the chloroform extracts and wash the stem of the funnel and the
filter with 10 mL of hot chloroform. Add the washings to the flask.
6. Evaporate the chloroform from the extract on a water bath under the
hood.
7. Using a buret, add 20 mL of 0.02 N H2SO4 and mix with the alkaloidal
extract. Transfer the mixture into an erlenmeyer flask.
8. Add 3 drops of methyl red T.S.
9. Titrate the excess acid by titrating it with 0.02 N NaOH until yellow.
81
Data and Results:
A. Data Obtained
Data Result
Weight of Coffee powder (g)
Normality of H2SO4
Volume of H2SO4 consumed (mL)
Normality of NaOH
Volume of NaOH consumed (mL)
% Caffeine content
B. Calculations:
(label properly)
Questions:
1. Identify the chemicals used in the experiment and indicate their
individual use.
82
3. Discuss how alkaloids are separated from other constituents.
Conclusion:
83