Name - Shatanshu Raj Student ID: SE21UCSE199 Batch Number: A4

Experiment 2: Determination of surface tension of a liquid by drop-count method

Objective: Determine the concentration (in volume percent) of an unknown solution of

methanol using surface tension measurements.

Procedure:

Q1. Describe in your own word how to conduct the experiment with all the necessary details.

Chemicals required

- Distilled water

- Standard solution of methanol 20% (v/v)

- Solution of methanol with unknown volume percent concentration.

Apparatus and laboratory glassware required

- Pipette pump - 10 mL Graduated cylinder

- Stand - 50 mL Graduated cylinder
- Balance - 4 Beakers
- Stalagmometer - 500 mL Beaker for waste

After we set up all the apparatus required, we dilute our 20% methanol with water to the
2.5%, 5%, and 10% concentrations.

Now we fix the stalagmometer firmly (filled with water) and keep a beaker (weighted before)
under it and then slowly release the water with the rate of 10-15 drops per minute. The
number of drops are counted until all the water is drained into the beaker, and then we weigh
the beaker again to calculate average mass of one drop of water.

Repeat this for all the concentration of methanol (20%, 10%, 5%, 2.5%) and for the unknown
solution. After we get the values for all average mass of on drop of each diluted methanol and
of our unknown solution, we calculate the surface tension.

The surface tension of one liquid can then be calculated with the relation :
!!"#$"% "
!&'()*
= "!"#$"% , where 𝑚#$%&$' and 𝑚()*+, are the masses of one drop of liquid and the mass
&'()*
of one drop of water respectively.

Results and interpretation:

Q2. How would the surface tension behave with the increasing concentration of Methanol?
How would the number of drops dissipated from the stalagmometer vary with varying
concentration?

As the concentration of Methanol is increased, the mass percentage of methanol is increased,

due to this the average mass of one drop of methanol also increases and as per the relation
!!"#$"% "
!
= "!"#$"% , the surface tension of Methanol increases.
&'()* &'()*
Name - Shatanshu Raj Student ID: SE21UCSE199 Batch Number: A4

Since we have a varying concentration, the less concentrated the solution is, the more drops
we will get per minute and vice-versa. Given the fact that release pressure of solution from
stalagmometer is kept constant throughout.

Further Questions:

Q3. How will the surface tension change upon increasing temperature?

The surface tension of liquids generally decreases with increase of temperature and becomes
zero at critical temperature (when meniscus between the liquid and the vapour disappears).
The decrease in surface tension with increase of temperature is due to the fact that with
increase of temperature, the kinetic energy of the molecules increases and hence
intermolecular attraction decreases.
Name - Shatanshu Raj Student ID: SE21UCSE199 Batch Number: A4

Experiment 4: To Prepare buffer solutions and to test their resistance to pH change

Objective: The aim of this experiment is to prepare some useful buffer solution that are
frequently used in chemistry and biology and to test their pH resistance.

Procedure:

Q1. Describe in your own word how to conduct the experiment with all the necessary details.

Chemicals required for citrate buffer

- Citric acid monohydrate

- Trisodium citrate dehydrate

Apparatus and glassware required

- Pipet pump - Two 5 ml pipette
- pH meter - Two 50 ml beaker
- Wash bottle -25ml Beaker for pH
- 500 mL Beaker measurement
- Two 250 ml beaker - Two clean plastic droppers
- Two 100 ml volumetric flask

Here, we will make a citrate buffer solution.

To do this we first prepare 100 mL of two standard solutions and then leave then for
some time so that they attain room temperature.

- 0.1M Citric acid monohydrate (C6H8O7•H2O, MW = 210.14)

- 0.1M Trisodium citrate dihydrate (C6H5O7Na3•2H2O, MW = 294.12)
After they attained room temperature, Prepare 25.0 ml solution for each of citrate
buffer, by mixing the above standard solutions. Take it in a 50 mL beaker and measure
the pH of each of the buffer solutions using the pH meter. Then we need to preserve
any of the two buffer solutions that we have prepared, for further testing and label as
buffer 1 and 2. While making a note of the room temperature.
After we are done making the buffer solution, we now test the resistance of buffer
towards addition of acid and base. To do this we first measure the pH once again of 25
ml of buffer 1 using the pH meter. Then to buffer 1, add 5 drops of 0.1M HCl, mix well
and measure the pH, then repeat by adding a further 5 drops of acid and measuring the
pH each time until we have added a total of 25 drops of 0.1M HCl. Do the same with
buffer solution 2 by adding drops of supplied 0.1M NaOH solution.
Now we make blank measurements using distilled water, we do this through repeating
the above procedure by taking 25 ml of distilled water and measuring the pH again, and
then compare the obtained results on a buffer solution with that of water by plotting
the measured pH for pure water and buffer solution as a function of drops of HCl added.
Name - Shatanshu Raj Student ID: SE21UCSE199 Batch Number: A4

Results and interpretation:

Q2. What difference would be observed while adding acid/base to the water compared
to buffer solution?

When we have acid/base to water their pH reduce rapidly but A buffer is an aqueous
solution containing a weak acid and its conjugate base or a weak base and its conjugate
acid. A buffer’s pH changes very little when a small amount of strong acid or base is
added to it. It is used to prevent any change in the pH of a solution, regardless of solute.
Buffer solutions are used as a means of keeping pH at a nearly constant value in a wide
variety of chemical applications.

Further question:

Q3. What causes buffering action in these solutions?

When some strong acid (more H+) is added to an equilibrium mixture of the weak acid
and its conjugate base, the equilibrium is shifted to the left, in accordance with Le
Chatelier’s principle. This causes the hydrogen ion (H+) concentration to increase by less
than the amount expected for the quantity of strong acid added. Similarly, if a strong
base is added to the mixture, the hydrogen ion concentration decreases by less than the
amount expected for the quantity of base added. This is because the reaction shifts to
the right to accommodate for the loss of H+ in the reaction with the base.
Name - Shatanshu Raj Student ID: SE21UCSE199 Batch Number: A4

Experiment 5: UV-visible spectroscopy

Objective: To Determine the concentration of a metal ions in a solution using complexometric

spectroscopy method.

Procedure:

Q1. Describe in your own words how to conduct the experiment with all the details.

Apparatus and glassware required

- Two 50 mL volumetric flask

- Ten 25 mL (or 50 mL) beakers
- One 250 mL beaker
- 500 mL beaker
- Watch glass
- Funnel
- Spatula
- 5 mL Volumetric pipette
- Two 2mL graduated pipettes
- Wash bottle with distilled water
- Dropper
- Two pipette pumps

To find the concentration of metal ions in a solution using complexometric spectroscopy

method we need a calibration curve, which is obtained by measuring the absorbance of
solution of known molarity in order to determine the molarity of the unknown solution 1.

Now to continue with our experiment we use EDTA as a ligand and prepare 50.0 ml of 0.2M
standard solution of EDTA by using the given salt.

After this we either need to prepare 5 standard solution of 0.020 M Cu(SO4) or of 0.050M
Co(NO3)2 by mixing them with EDTA provided and calculate the molarity from their respective
absorbance values. As we are done with our standard solution of known molarity, we now
pipette 8.0 mL of unknown solution and add 2.0 mL of EDTA solution to it and again we
prepare the same standard solution but this time we replace water with EDTA solution and
then Deduce the molarity of the unknown solution.

For the final part after we are done with our calculations we just plot our calibration curves
by obtaining the spectrum of most concentrated solution and by measuring the absorption at
wavelengths of maximum absorption for the 5 solutions that we made earlier, along with our
unknown solution with EDTA.
Name - Shatanshu Raj Student ID: SE21UCSE199 Batch Number: A4

Results and interpretation:

Q2. How are the absorbance and concentration related? Explain in detail.

Absorbance and concertation are related to each other through the Beer–Lamberts Law,
stating that absorbance has a proportional relationship to concentration. As the
concentration goes up more radiation is absorbed and the absorbance goes up and the Beer-
lambert equation is,

𝐴$ (𝜆) = 𝜀$ (𝜆)𝐶𝐿
Here ε- (λ) is the molar absorptivity of the substance at wavelength λ, and L is the path length
of the cell containing the solution.

Further questions:

Q3. Draw the structure of EDTA-Cu or EDTA-Co octahedral complexes, and

qualitatively the change in wavelength when adding EDTA using Crystal Field Theory.

Molecular Formula of EDTA – C is C10H14CoN2O8

and the structure is,

Crystal field theory (CFT) describes the breaking of

orbital degeneracy in transition metal
complexes due to the presence of ligands. CFT
qualitatively describes the strength of the metal-
ligand bonds. Based on the strength of the metal-
ligand bonds, the energy of the system is altered.
In an octahedral complex, there are six ligands
attached to the central transition metal. The d-
orbital splits into two different levels. The bottom
three energy levels are named dxydxy, dxzdxz,
and dyzdyz (collectively referred to as t2gt2g). The
two upper energy levels are named dx2−y2dx²−y², and dz2dz² (collectively referred to
as egeg), and in this octahedral comple the electrons are attracted to the axes. Any orbital
that has a lobe on the axes moves to a higher energy level. This means that in an octahedral,
the energy levels of egeg are higher (0.6∆o) while t2gt2g is lower (0.4∆o).
Name - Shatanshu Raj Student ID: SE21UCSE199 Batch Number: A4

Experiment 7: Determination of hardness of water

Objective: Determine the total hardness of sample water, the permanent hardness, the
temporary hardness and the molarity of Magnesium and Calcium.

Procedure:

Q1. Describe in your own words how to conduct the experiment with all the details

Chemicals provided
- Ethylene diamine tetra acetic acid (EDTA) MW = 372.24
- Standard solution of Mg(NO3)2 of concentration 0.01M
- Indicator Eriochrome Black T (EBT)
- Ammonia buffer solution, pH=10.
- Sample water
- Ammonium oxalate
Apparatus and glassware required

- Burette on stand - 2 funnel - Two watch glasses

- Volumetric flask 50 mL
- Volumetric flask 250 mL
- Pipette pump
- 10 mL volumetric pipette
- Spatula
- 100 mL Conical flask
- Dropper
- 250mL Conical flask
- 500 ml Beaker
- Two 250 mL beakers

Prepare 250.0 mL of 0.005M solution of EDTA (MW=372.24) in a volumetric flask. Fill the
burette with this solution. Now we need to do standardisation of our EDTA solution as it is
not pure, for this we have to first pipette out 10.0 mL of 0.01M provided solution of Mg2+ and
taken into a 100mL conical flask. About 2mL of ammonia buffer is then added using the
dropper under the hood, as well as 2 drops of EBT indicator. The mixture is shaken well and
titrated with the prepared 0.005M EDTA solution until the wine red colour changes to blue
and then the standard molarity of EDTA solution is calculated.
Now we determine the total hardness, we do this this by repeating the previous titration and
replacing Mg2+ solution with 10.0 mL of sample water in the conical flask. Using the same
procedure of titrating we standardise EDTA solution with water, till we observe a colour
change. The total hardness of water is calculated by calculating the molarity and using the
provided formula,
Total Hardness = Molecular weight of Mg(NO)3 x Molarity of Sample water
After we get total hardness of water, we find the permanent hardness. For this, the titration
is repeated with 10.0 mL of supplied boiled sample water using the same procedure and then
calculate it using the formula,
Name - Shatanshu Raj Student ID: SE21UCSE199 Batch Number: A4

Permanent Hardness = Molecular weight of Mg(NO)3 x Molarity of boiled water

Now we, determine the molarity of Mg2+ in total hardness of water. We do this by adding
about 0.04g of ammonium oxalate to about 25 mL of sample water in a beaker. The beaker is
gently shaken by hand for 30s. The content is then filtered, 10.0 mL of the filtrate is titrated
as previously. The total magnesium hardness is determined. From this value the total calcium
hardness is calculated.
Results and interpretation:

Q2. What would happen to the hardness of water after it is boiled? According to you what is
the role of ammonium oxalate?
Boiling the water causes the precipitation of solid calcium carbonate or solid magnesium
carbonate. This removes the calcium ions or magnesium ions from the water, and so removes
the hardness. Therefore, hardness due to hydrogen carbonates is said to be temporary.

Here, ammonium oxalate (C2H8N2O4) is used a reducing agent and selectively precipitates Ca2+
ions, which can be removed by filtration.

Further questions:
Q3. Specify if the water is soft, moderately hard, hard or very hard.
Softness of water is can be determined by the value it’s ranging from.
For <60, it’s soft.
For 61-120, It’s moderately hard.
For 121-180, it’s hard.
For >180, it’s very hard.