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Undergraduate

Chemical Laboratory-I
Manual (Part A)
2018

Tapan Kanti Paine

School of Chemical Sciences


Indian Association for the Cultivation of Science
Kolkata

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UG Chemistry Lab Experiments
(Semester-I of 2018)

(A) Titrimetric Analysis and Acid-Base Titration

1. Introduction to laboratory glassware, their use and calibration


2. Preparation of solutions of different Molarity/Normality of titrants and
their standardization
3. Determination of the normality of hydrochloric acid by a standard
solution of sodium carbonate
4. Determination of the amount of sodium carbonate and sodium hydroxide
in a mixture
5. Determination of the purity of aspirin tablets by acid-base titration
6. Analysis of a mixture of carbonate and bicarbonate

(B) pH Metry

7. Preparation of buffer solutions of different pH


8. pH Metric titration of (i) strong acid vs strong base (ii) weak acid vs
strong base
9. Determination of dissociation constant of a weak acid

(C) Surface Tension and Viscosity

10. Determination of surface tension


11. Variation of surface tension of detergent solutions with concentration
12. Determination of viscosity of aqueous solution of polymer, ethanol and
sugar at room temperature
13. Variation of viscosity of sucrose solution with the concentration of solute

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Experiment 1:
Introduction to laboratory glassware, their use and calibration

(a) Common Laboratory Glassware and Volumetric Glassware (demo)

(b) Calibration of Glassware


Glassware is commonly calibrated using a liquid of known, specific density, and
an analytical balance. The procedure is to determine the mass of liquid the
glassware will hold, and to divide this mass of liquid by the density of the liquid,
obtaining the corresponding volume of liquid. Density is affected by
temperature, so it is necessary to measure the liquid temperature and look up
appropriate density values.

Volumetric flasks
1. Take 3 dry volumetric flasks of appropriate size (25.00 or 50.00 mL)
along with their stoppers. Label the flasks (1, 2 and 3).
2. After the analytical balance has been leveled and calibrated, tare the
balance. Determine the mass of each flask and its stopper, and record
these masses in your notebook. Make sure that you tare the balance before
massing each flask.
3. Dispense a suitable volume of deionized water into a beaker, and measure
and record the temperature of the deionized water. Check the relation
between temperature correct density of water. Fill each of the flasks with
deionized water to the fill line. Mass the filled flasks, making sure to
record the masses of the filled flasks in your notebook.
4. Calculate the corresponding volumes of water contained by each of the
flasks, and calculate the mean and sample deviation for each flask. When
you are done, you should have a data table similar to that shown below:

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Flask 1 Flask 2 Flask 3

Tare mass, g

Filled mass, g

Mass of water, g

Volume water, mL

Pipets
1. Take 3 dry pipets of appropriate size (10.00 or 25.00 mL). Label the
pipets (1, 2 and 3).
2. Measure the mass of a suitably sized beaker (~50 mL) on the analytical
balance, and record the mass in your notebook.
3. Rinse the first pipet 3 times with deionized water by filling the pipet to
the fill line, and discarding the rinse. Finally, fill the pipet to the fill line,
wipe excess water from the outside of the pipet and dispense this liquid
into the beaker. Measure and record the mass of beaker and water,
4. Calculate the corresponding volume of water delivered by each pipet, and
calculate the mean and sample deviation for each pipet.

Pipet 1 Pipet 2 Pipet 3

Mass of water, g

Volume water, mL

Burets
1. Select a suitably sized buret (25.00 or 50.00 mL) and carefully clean and
rinse the buret with deionized water.
2. Measure the mass of a suitably sized beaker (~50 mL) on the analytical
balance, and record the mass in your notebook.
3. Obtain a volume of deionized water (100 - 200 mL), and measure the
temperature of the water. Fill the buret with deionized water to the 0.00
mL line.

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4. Dispense a portion of deionized water from the buret into the beaker. The
portion size depends on the size of the buret: ~5 mL for a 25.00 mL buret,
or ~10 mL for a 50.00 mL buret. Record the indicated volume from the
buret in you notebook.
5. Determine the mass of water dispensed using the analytical balance.
Record this value in your notebook.
6. Repeat steps 4 and 5 until the 25.00 mL (or 50.00 mL, depending on the
size of the buret) mark has been reached. For each TOTAL volume of
water dispensed, record the TOTAL mass.
7. Now you can discard the water in the beaker.
8. For each set of calibration data, determine the volume of water dispensed
by dividing the total mass of water dispensed by the density of water at
that temperature. When you have finished each calibration, you should
have a data set similar to that shown below

Indicated volume Mass of water Calculated volume of


(buret), mL dispensed, g water, mL

9. Determine the difference in volumes by subtracting the calculated volume


of water from the indicated volume of water.

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Experiment 2:
Preparation of solutions of different Molarity/Normality of
titrants and heir standardization

Solutions of accurately known strength are called standard solutions


A standard solution contains a known weight of reagent in a definite volume of
solution
Molar solution
Molar solution is one, which contains one molecular weight of the reagent in
one litre of the solution. Molarity is expressed as M.
Normal solution
Normal solution is one, which contains one equivalent weight of the reagent in
one litre of the solution. Normality is expressed as N.
Equivalent weight of acid = Molecular weight/ No. of replaceable H+ ions

Standards in Titrimetry
• Primary Standards - materials that can be weighed out exactly
• Secondary Standards - standardized against primary standards
• Standard Solutions - made up approximately, then standardized

Requirements of Primary Standard


• Highest purity…
• High molecular/formula weight
• Stable to drying
• Readily available (and cheaply)
• Not deliquescent (Phenomenon of a substance absorbing so much moisture
from the air that it ultimately dissolves in it to form a solution) or hygroscopic.

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(a) Preparation of N/10 NaOH solution
Molecular weight of NaOH = 40
Acidity (number of replaceable OH group) = 1
Equivalent weight of NaOH = 40
Therefore, 4 g of NaOH dissolved in one litre of solution will give N/10 NaOH
solution.
Procedure
Weigh quickly 4 g NaOH in a beaker (as it is hygroscopic) and dissolve it in
distilled water (preferably CO -free). Transfer the contents and the washings to a
volumetric flask (1 litre). Cool and then make volume up to the mark. Shake
well and standardize this solution against N/10 oxalic acid using
phenolphthalein as an indicator. Label it as 0.1 N NaOH solution

(b) Preparation of N/10 oxalic acid

Oxalic acid (COOH)2 .2H O is to be dissolved in one litre of distilled water to


get N/10 oxalic acid solution.

Procedure
Weigh accurately 6.3 g (COOH)2 .2H O and transfer it to a volumetric flask (1
litre), half-filled with distilled water. Shake well and make the volume up to the
mark. Label it as N/10 oxalic acid solution.

Note: If anhydrous oxalic acid (COOH)2 is available then dissolve 4.5 g of the
acid in one litre of distilled water to get 0.1 N oxalic acid solution.

(c) Standardization of NaOH solution:

1. Take a 50 mL buret and rinse it with distilled water. Finally, rinse it three
times with about 4 mL of your NaOH solution each time. Fill the buret with
NaOH solution and cover the top of the buret with plastic wrap until you are
ready to use it.

2. Take 10 mL of oxalic acid solution in an Erlenmeyer flask and add 2 drops of


phenolphthalein. Swirl the mixture to dissolve the. Read the buret to the nearest
0.01 mL, and titrate the oxalic acid with NaOH. The end point has been reached
when the pale pink color of the phenolphthalein persists for 30 seconds. Try to

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carry out the titration so that the last half-drop of NaOH causes the change in
color.

3. Repeat the titration and calculations until you have three determinations that
agree within accepted error limit.

4. Calculate the strength of NaOH solution.

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Experiment 3

(a) Determination of the normality of hydrochloric acid by a standard


solution of sodium carbonate (0.1N)

Theory:
Sodium carbonate reacts with hydrochloric acid according to the
following equation:
Na2CO3 + 2HCl = 2NaCl + CO2 + H2O
In other words, to neutralize all the carbonate, two equivalent of HCl should be
used and as such the equivalent weight of sodium carbonate = M.wt/2 =53
When one equivalent of HCl is added to the carbonate it is transformed into
bicarbonates.
Na2CO3 + HCl = NaHCO3 + NaCl Phenolphthalein (ph.ph)
And the pH of the solution changes form 11.5 (alkaline) to 8.3. When
phenolphthalein is used, it changes to colorless at the end of this stage as its
color range falls within the same zone. ph.ph (8.3-10).
When another equivalent of HCl is added to the solution of bicarbonate,
complete neutralization takes place and it is transformed into sodium chloride
and CO2 gas is evolved.
NaHCO3 + HCl = NaCl + H2O + CO2 Methyl Orange (M.O.)
The pH of solution changes from 8.3 to 3.8, which is near enough to the color
range of M.O. (3.1-4.4). If M.O. is used at this stage, the color of the solution
changes from yellow to red. It thus follows that ph.ph. is used in the
neutralization of HCl with sodium carbonate, the volume of acid used will be
equivalent to half of the carbonate, when methyl orange is used in this titration
the volume of acid used will be equivalent to all carbonate. Methyl orange is
generally used in this as ph.ph. is sensitive to carbon dioxide.

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Materials:
(i) Sodium carbonate solution (standard).
(ii) HCl solution of unknown normality.
Preparation of standard solution of Na2CO3 (0.1N):

1- Weigh out accurately 1.325 gm of A.R. Na2CO3 (should be dried in over


prior to use for conversion of any NaHCO3 in the sample)
2- Dissolve in small quantity of distilled water and transfer quantitatively to 250
ml measuring flask.
3- Complete to the mark and shake well.
4- Calculate the exact normality of Na2CO3 solution.
Weight required = Normality x eq.wt. x volume in liter.

Procedure:
1- Transfer 10 ml of the sodium carbonate solution with a pipette to a
conical flask then add one or two drops of M.O. to this solution.
2- Add the acid (HCl) from the burette gradually with continuous stirring of
the solution in the conical flask, and near the end point, the acid is added
drop by drop. Continue the addition of the acid till the color of the
solution passes from yellow to orange.
3- Repeat the experiment three times and tabulate your results then take the
mean of the three readings.
4- Repeat the experiment using phenolphthalein which changes its color
from red to the colorless at the end point. Compare the results in this case
with those in the case of M.O.

Calculations:
 In case of M.O.
Suppose that the volume of HCl is V1 and its normality is N1 while V2 is
the volume taken from sodium carbonate and N2 is its normality.
The volume of HCl (from burette) ≡ all carbonate = V1

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N1 V1(HCl) = N2 V2(Na2CO3)
Or N1= N2 V2/V1
 In case of ph.ph.
The volume of HCl (from burette) ≡ 1/2 carbonate
The volume of HCl ≡ all carbonate = 2V1
N12V1 = N2 V2
Or N1 = N2 V2 / 2V1
And as the strength in gm/L = normality x eq. wt.
Strength of HCI = N1 x 36.5 g/L

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Experiment 4:

Determination of the amount of sodium carbonate and sodium


hydroxide in a mixture

(a) Determination of the strength and normality of sodium hydroxide


solution by a standard solution of hydrochloric acid

Theory:
HCl reacts with sodium hydroxide according to the following equation:
HCl+ NaOH = NaCl + H2O
The eq.wt. of both the HCl and NaOH is equal to their molecular weights and so
both the acid and alkaline are strong, any indicator may be used.
Materials:
HCl solution (standard).
NaOH solution of unknown normality.
Procedure:
a- Prepartion of sodium hydroxide solution:
1- Weigh about 4.0 gm of A.R. NaOH.
2- Dissolve in small volume of distilled water and transfer to one-liter
measuring flask.
3- Complete to the mark with distilled water, place the stopper on the
bottle and thoroughly mix the solution by shaking the bottle.
b- Standardization of the resulting NaOH solution:
1- Transfer with a pipette 10 ml of NaOH solution to a conical flask
then add one or two drops of M.O., add the standard HCl solution
from the burette till the end point. (the color changes from yellow
to reddish orange)
2- Repeat the experiment three times and tabulate your results.
3- Repeat the experiment using ph.ph. and Compare the result with
those obtained With M.O.

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Calculations:
In both cases of M.O. and ph.ph.
use the relation :
N1V1(HCl) = N2 V2(NaOH)
In order to deduce the normality of NaOH
Strength of NaOH = N2 x 40 (eq.wt.) = g/L.

(b) Determination of the amount of sodium carbonate and sodium


hydroxide in a mixture

Theory:

1- When a known volume of the mixture is titrated with HCl in presence of


phenolphthalein., the acid reacts with all the sodium hydroxide and with only
half of the carbonate.
V1 = all hydroxide + 1/2 the carbonate
2- When a known volume of the mixture is titrated with HCl in presence of
M.O., the acid reacts with all the hydroxide and all the carbonate.
V2 = all hydroxide + all carbonate
Volume of HCl = 1/2 carbonate = V2 – V1 = V ml
Volume of HCl = all carbonate = 2V ml
Volume of HCl = NaOH = V2 - 2V ml
Procedure 1:
1- Transfer with a pipette 10 ml of the mixture to a conical flask, and add one or
two drops of ph. ph.
2- Add the acid from the burette till the solution becomes colorless.
3- Repeat the experiment twice or three times and tabulate your results.
 The volume of acid in the case is V1 and is equivalent to all the hydroxide
and half the carbonate.
4- Repeat the experiment with methyl orange until the color of the solution is
changed to faint red.

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5- Repeat the experiment twice or three times and tabulate your results.
 The volume of acid in the case is V2 and is equivalent to all the hydroxide
and all the carbonate.
6- Calculate the strength of the sodium hydroxide and the sodium carbonate in
the mixture.

Calculations1:
 In the case of Na2CO3:
N1 x 2V = N (Na2CO3) x 10
Strength Na2CO3 = N (Na2CO3) x 53 g/L
 In the case of NaOH:
N1 x (V2 - 2V) = N (NaOH) x 10
Strength NaOH =N (NaOH) x 40 g/L

Procedure 2:
1- Transfer with a pipette 10 ml of the mixture to a conical flask, and add one or
two drops of ph. ph.
2- Add the acid from the burette till the solution becomes colorless.
 The volume of acid in the case is V1 and is equivalent to all the hydroxide
and half the carbonate.
3- Then add two drops of methyl orange to the same conical flask and continue
titration to the faint red color or the orange color.
 The volume of acid in the case is V2 and is equivalent to the second half
of carbonate.
3- Repeat the experiment three times and tabulate your results.
4- Calculate the strength of the sodium hydroxide and the sodium carbonate in
the mixture.

Calculations 2:
 In the case of Na2CO3:

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N1 x 2V2 = N (Na2CO3) x 10
Strength Na2CO3 = N (Na2CO3) x 53 g/L
 In the case of NaOH:
N1 x (V1 - V2) = N (NaOH) x 10
Strength NaOH =N (NaOH) x 40 g/L

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Experiment 5:
Determination of the purity of aspirin tablets by acid-base
titration

This experiment is designed to illustrate techniques used in a typical indirect or


back titration. Back titration is performed for analysis where detection of end-
point is difficult in direct titration. Many reactions are slow or present
unfavorable equilibria for direct titration. Aspirin is a weak acid that also
undergoes slow hydrolysis; i.e., each aspirin molecule reacts with two hydroxide
ions. To overcome this problem, a known excess amount of base is added to the
sample solution and an HCl titration is carried out to determine the amount of
unreacted base. This is subtracted from the initial amount of base to find the
amount of base that actually reacted with the aspirin and hence the quantity of
aspirin in the analyte.

Preparation of Approximate Acid Solution (~ 0.1M HCl) and


standardization with NaOH

1. Prepare 250 mL of 0.1M HCl in a bottle.


(Concentrated reagent grade HCl has a density of 1.188 g mL–1 and is 37 wt %.
Measure the required volume of concentrated HCl using a graduated cylinder.
Gradually add the acid to the water in your bottle, mixing well (remember,
always add acid to water, not water to acid). Add more distilled water, mixing
thoroughly with each addition, until the total solution volume is ~ 250 mL. You
do not have to measure the quantities accurately because you are going to
standardize this solution in the next steps to determine its actual concentration.

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2. Clean, rinse, and fill your burette with your ~0.1 M HCl solution. To each of
three clean, labelled Erlenmeyer flasks, add 50 mL distilled water and three
drops of phenolphthalein indicator. Use your HCl burette to add approximately
35, 40 and 45 mL of acid to flasks #1, #2 and #3, respectively, recording exactly
how much acid is added to each flask within 0.01 mL. Swirl gently to mix.

3. Clean, rinse, and fill your second burette with the ~0.1 M NaOH solution that
you standardized last week. Titrate the three HCl flasks with the NaOH to the
phenolphthalein endpoint.

Sample Preparation

4. Accurately record the weight of a group of three aspirin tablets so that you
can determine an average tablet weight. Use a mortar and pestle to crush enough
tablets to produce ~ 1 g tablet powder.
5. Using a clean dry weighing bottle, weigh accurately, by difference, triplicate
~0.3 g samples of tablet, into labeled 250 mL Erlenmeyer flasks. To each flask,
add 20 mL of ethanol (measure by graduated cylinder) and three drops of
phenolphthalein indicator. Swirl gently to dissolve. (Aspirin is not very soluble
in water — the ethanol helps the aspirin dissolve. Note that an aspirin tablet
contains other compounds in addition to aspirin. Some of these are not very
soluble. Your solution will be cloudy due to insoluble components of the tablet.)

Aspirin Titration with base

6. Clean, rinse, and fill a burette with the ~0.1 M NaOH solution that you
standardized following the experiment done before. Titrate the first aspirin
sample with NaOH to the first permanent cloudy pink colour.

7. The aspirin/NaOH acid-base reaction consumes one mole of hydroxide per


mole of aspirin. The slow aspirin/NaOH hydrolysis reaction also consumes one
mole of hydroxide per mole of aspirin, and so for a complete titration you will
need to use a total of twice the amount of NaOH that you have already used,
plus you will add some excess NaOH to ensure that you really have reacted
with all of the aspirin in your sample (adding excess reactant drives the
equilibrium towards products — Le Chatelier’s principle).
Calculate how much extra NaOH you will need to add, following this reasoning:
The volume of base to add for the hydrolysis reaction is equal to the volume of
base you have already used to titrate to the acid-base endpoint in Step 6 plus an
additional 10 mL of excess base. (For example: if you used 26 mL of base in
the previous step, the volume of base you would add now would be 26 + 10 = 36
mL. Thus, you would have added a total of 26 + 26 + 10 = 62 mL of base.)

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Use your burette (not a graduated cylinder) to add the appropriate amount of
extra NaOH to each of your three sample flasks. Record the total volume of
NaOH added to each flask within 0.02 mL.

Heating the reaction to completion

8. Add two or three boiling chips to each flask and heat in a water bath to speed
up the hydrolysis reaction. Avoid boiling, because the sample may decompose.
While heating, swirl the flasks occasionally. After 15 minutes, remove samples
from the water bath and cool for 5 minutes.

9. If the solution is colourless, add a few more drops of phenolphthalein. If it


remains colourless, add 10 mL more of the base and reheat. (Don't forget to add
this additional volume of base to the previously recorded total volume.)

Back titration with acid

10. The only base remaining in each flask will be excess base that has not
reacted with the aspirin. Using your burette with your ~0.1 M HCl solution,
titrate the excess base in each flask with HCl until the pink colour just
disappears. The endpoint is best described as “cloudy white”.

11. Using the volume of HCl needed to back-titrate each aspirin flask and the
average HCl concentration, calculate the number of moles of excess NaOH left
in each flask after the reaction with aspirin.

12. From the total number of moles of NaOH added to the sample, and the
number of moles of excess NaOH left after the reaction was complete, calculate
the number of moles of base that reacted with aspirin.

13. Determine the number of moles of aspirin in each of your samples. (Don’t
forget the factor of two.)

14. Calculate the mass of aspirin in each of your samples. Using the mass of
tablet you weighed into each sample, calculate the weight percent of aspirin in
the tablets.

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Experiment 6:

Analysis of a Mixture of Carbonate and Bicarbonate

Purpose: You will analyze a sample for total alkalinity and then determine the
individual amounts of carbonate and bicarbonate.

Background
You will be given a mixed sample consisting of a carbonate (Na2CO3) and a
bicarbonate (NaHCO3). You will perform two titrations to determine three
different quantities:
1. Total alkalinity=[HCO3-]+2[CO32-]. For these samples, this is approximately
the amount of base that reacts with an added acid, hence the term “total
alkalinity”
2. the original amount of carbonate and bicarbonate present in your sample.

To determine total alkalinity, you will titrate your sample with the standard
hydrochloric acid using a bromocresol green end point. The reactions are:
HCO3-(aq) + H+(aq) ---H2CO3 (aq)
CO32-(aq) + 2H+(aq) --H2CO3(aq)
In this first titration, there is no way to differentiate between the second and first
reactions, so the endpoint of the reaction is for both of the reactions, together. In
the second step, you will determine the original carbonate concentration of your
unknown by exploiting a number of methods, including selective precipitation.
You will treat a fresh aliquot with an excess of the standard sodium hydroxide
converting all HCO3- to CO32-:
HCO3-(aq) + OH-(aq) -CO32-(aq) + H2O
Your sample then consists entirely of CO32-, which you will precipitate by
adding excess barium chloride:
Ba2+(aq) + CO32-(aq)--BaCO3(s)
The excess NaOH is then immediately titrated with standard hydrochloric acid
to determine how much bicarbonate had been originally present in the sample.
From this value and the total alkalinity, the original carbonate concentration can
be easily calculated.

Reagents

1. phenolphthalein indicator
2. bromoscresol green indicator
3. standardized ~0.1M sodium hydroxide
4. commercially standardized 0.1M hydrochloric acid
5. 10 wt% barium chloride solution

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6. Unknown carbonate/bicarbonate mixture (store in a dessicator; do not heat).

Procedure

1. Record the mass of your unknown. Use a funnel to transfer your unknown
into a 250mL volumetric flask and rinse your container and flask with CO2-free
water to ensure quantitative sample transfer.

2. Total alkalinity: Pipet a 25.00mL aliquot of unknown into a 125mL


Erlenmeyer flask and perform a rough titration with standard 0.1M HCl to a
bromocresol green (3 drops) endpoint. Perform three careful replicate titrations.

3. Bicarbonate content: Transfer another 25.00mL of unknown and 50.00mL


of your standard 0.1M NaOH into a 125mL flask. Swirl and add approximately
10mL of 10wt% barium chloride. Swirl again to precipitate barium carbonate.
Add 3 drops of phenolphthalein indicator and roughly titrate to endpoint with
0.1M HCl. Perform 3 careful replicate determinations.
4. Using the mean values of your replicate determinations, calculate the
composition (including standard deviation error) of your sample.

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