SOME

BASIC CONCEPTS REQUIRED FOR THIS COURSE:

q  What is (tra(on?
q  Quan(ta(ve analysis and qualita(ve analysis?
Qualita've Analysis (iden(fica(on) provides informa(on about the iden(ty of species or
func(onal groups in the sample (an analyte can be iden(fied).
Quan'ta've Analysis provides numerical informa(on of analyte (quan(tate the exact
amount or concentra(on).
q  What is solu(on?
q  What is concentra(on?
The concentra(on of a solu(on is a measure of the number of par(cles of the solute in the
solvent.
q  What is primary standard and secondary standard substances?
A primary standard is a reagent that is extremely pure, stable, has no water of hydra(on,
and has a high fixed molecular weight. K2Cr2O7, C2H2O4. 2H2O, Na2CO3 etc.

q  What is the characteris(c of primary and secondary standard substances?
A primary standard is a chemical or reagent which has certain proper(es such as (a) It is
extremely pure, (b) Highly stable (c) It is anhydrous (d) It is less hygroscopic (e) Has very high
molecular weight (f) Can be weighed easily (g) Should be ready to use and available (h)
Should be preferably non toxic (i) Should not be expensive.


q  What is indicator?
q  What kinds of indicators are
used in case of (tra(on of
I.  Weak acid and strong base
II.  Strong acid and weak base
III.  Strong acid and strong base
IV.  Weak acid and weak base

pH range 3.2-4.4

pH range 8.2- 10.0

Conductometric 'tra'on between weak base and weak acid:

Conductance Acid (H+)

Base (OH-)
q  What is end point?
q  What is weak acid and strong acid?
q  What is pH of solu(on?
q  What is pOH of the solu(on?
q  What is buffer solu(on?
q  How can you calculate the pH of a buffer solu(on?
q  What is molarity?
q  What is Normality?
q  What is molality?
q  Which depends temperature molarity or molality? Explain why?
q  What are the different units of concentra(on?
q  How do you prepare a 1 M/N HCl solu(on? Density of HCl: 1.48 g/ml Molecular weight
of HCl: 36.5g / mole Concentra(on of HCl stock: 36%.
The moles of HCl needed
Moles of HCl = 1L HCl × 1 mol HCl / 1L HCl = 1 mol HCl
The mass of HCl needed
Mass of HCl = 1mol HCl × 36.46 g HCl / 1mol HCl= 36.46 g HCl
The mass of solu(on required
Mass of soln = 36.46g HCl × 100 g soln / 36g HCl = 101.30 g soln
The volume of solu(on required
Volume of soln = 101.3g soln × 1 mL soln / 1.18g soln = 68.5 mL soln
To prepare 1M/N HCl, dissolve 68.5ml of 36% solu(on into 931.5ml of dis(lled H20.

q  How do you prepare 100 mL 0.1 N HCl solu(on from 10mL 9.4 N HCl solu(on?
q  How do you prepare 0.1 M Na2S2O3 solu(on?
q  How do you prepare 0.1 N KMnO4 solu(on?

N (normality) describes a solu(on that contains 1 gram equivalent weight (gEW) per
liter solu(on. An equivalent weight is equal to the molecular weight divided by the
valence (here it gets a lidle tricky, for acids and bases it refers to the number of H+ or
OH-).
In the case of KMnO4, equivalent wt is reac(on specific. When KMnO4 is used in acid
medium as oxidiser, 5 electrons are gainedby Mn atom. So equivalent wt of KMnO4 in
acid medium = Molecular wt/no.of electrons gained in redox reac(on = 158/5 =31.6. So
for 0.1N KMnO4 solu(on, you have to dissolve 3.16g KMnO4 in 1L water.
In alkaline or neutral medium, reac(on of KMnO4 is different and Mn gains 3 electrons
in redox reac(on. So, for alkaline medium redox (tra(ons, equivalent wt of KMnO4 will
be 158/3 = 52.6. So for 0.1N KMnO4 solu(on in alkaline medium redox (tra(on,
dissolve 5.26g in 1L water.


q  How do you prepare 0.1 N K2Cr2O7 solu(on in acidic medium reac(on?
EXPT. NO.: l.
STANDARDIZATION OF NaOH SOLUTION WITH STANDARD OXALIC ACID SOLUTION:

Objec've:
1.  Prepara(on of different types of solu(on
2.  Calcula(on of concentra(on of prepared solu(on
3.  Standardiza(on of prepared solu(on
4.  Understanding the process of (tra(on
5.  Understanding the selec(on of indicator during (tra(on.

PRINCIPLE:
Sodium hydroxide is deliquescent (absorbs moisture from the atmosphere) solid. It
cannot be weighed accurately. Therefore, it is not possible to prepare a standard
solu(on of sodium hydroxide of accurately known concentra(on by weighing NaOH. A
sodium hydroxide solu(on of approximate concentra(on (0.1 M) is to be prepared. It is
then standardized by (tra(ng it against an accurately weighed sample of oxalic acid,
which is a primary standard acidic substance.

PREPARATION OF N/10 OXALIC ACID SOLUTION:
Transfer 0.63 g. of pure Oxalic Acid (HOOC-COOH. 2H20) in a 100 mL volumetric flask
and then dissolve it with dis(lled water upto the mark. Normality of the prepared acid
solu(on will be calculated as



PROCEDURE:
Take 10 mL of supplied NaOH solu(on in a conical flask by means of a pipede and
dilute it to about 50 mL. Add one drop of Phenolphthalein indicator to the solu(on.
Then add Standard Oxalic Acid solu(on drop by drop from a burede. Shake the flask
frequently while adding the acid solu(on. Stop the addi(on of oxalic acid solu(on as
soon as the pink colour of the solu(on just disappears. Note the burede reading. The
burede reading should be taken carefully at the lower meniscus of the liquid.
Difference of the ini(al and final burede reading gives the volume of the acid added.
The process should be repeated at least twice. These should agree within ± 0.1 mL.
Calculate the normality of the supplied NaOH solu(on. Using the following rela(on.

Data and table:
Run No Vol. NaOH IBR(ml) FBR(ml) Diff. (ml) Avg.(ml)
1 10
2 10 10.0
3 10

Calcula'on:
Formulae = V acid × N acid = V base × N base

RESULTS and DISCUSSIONS

(i) Molarity of prepared NaOH solu(on……….N
(ii) Molarity of standardized NaOH solu(on……….N
(iii) Moles of NaOH in 100mL………..mol
(iv) Mass of NaOH in 100 mL…………g
Students should know:
r What is the normality of supplied solu(on?
r What are the molecular structure of phenolphthalein and oxalic acid?
r How does the indicator (phenolphthalein) work?
r At what pH does the indicator changes its color?
r Do you know why we see different color of different solu(ons?
 EXPT. NO. 2.
STANDARDIZATION OF HYDROCHLORIC ACID WITH STANDARD NaOH SOLUTION.

Objec've:
q  Introduce the concept of the analy(cal (tra(on.
q  Learn how to standardize strong acids and bases.
q  How to determine the purity of an impure weak acid.
q  To prac(ce the basic laboratory skills you need in order to perform accurate
q  and precise (tra(ons.

Principle:
Hydrochloric acid is a secondary standard substance and commercial HCl is very
concentrated. To obtain most standard acid solu(ons, a solu(on of an approximate
concentra(on is first prepared by dilu(ng the concentrated reagent. A HCl solu(on of
approximate concentra(on (0.1 M) is to be prepared. It is then standardized by (tra(ng it

against previouly stardarized sample of NaOH.



Experimental:
(a) Standardize the supplied NaOH solu(on as in Experiment No.1.
(b) Prepara'on of approximately N/10 Hydrochloric acid (HCI) solu'on.
Take about 1.2 - 1.3 mL conc. HCl in a 100 mL volumetric flask and add dis(lled water
upto the mark.

PROCEDURE:
Take 10 mL standard NaOH solu(on in a conical flask and dilute it to about 50 mL. Add 2
or 3 drops of Methyl Orange indicator to the solu(on. Then add previously prepared
(approx. N/l0) HCI acid solu(on drop wise from a burede. Shake the flask frequently
during addi(on of HCI acid. Stop addi(on of HCI acid solu(on as soon as the yellow color
of the solu(on just changes to orange. Note the burede reading. Repeat the process at
least two (mes and these should agree within ± 0.1 mL. Calculate the normality of the
dilute HCl and from there calculate the strength of commercial HCl.


Vbase × Nbase = Vdilute acid × Sdilute acid
(b) Vdilute acid × Sdil. acid determine = Vconc.acid taken × Nconc. acid to be determine

Data and table:
Run No Vol. NaOH IBR(ml) FBR(ml) Diff. (ml) Avg.(ml)
1 10
2 10 10.0
3 10

Calcula'on:
(a) Vbase × Nbase = Vdilute acid × Sdilute acid
(b) Vdilute acid × Sdil. acid determine = Vconc.acid taken × Nconc. acid to be determine

RESULTS and DISCUSSIONS

(i) Molarity of prepared HCl solu(on……….N
(ii) Molarity of standardized HCl solu(on……….N
(iii) Moles of HCl in 100mL………..mol
(iv) Mass of HCl in 100 mL…………g
Students should know:
r What is the normality of the supplied HCl solu(on?
r What is the molecular structure of methyl orange indicator?
r Can we use phenolphthalein instead of methyl orange here? Jus(fy your answer.
r At what pH does the indicator changes its color?
r Is it necessary to use buffer solu(on here? If not why?
Neutraliza(on reac(on between Na2CO3 and HCl acid takes place into two steps-

Na2CO3+ 2HCl => NaHCO3 + 2NaCl

NaHCO3+HCl =>NaCl + H2CO3

The ul(mate reac(on,
Na2CO3+ 2HCl =>2NaCl + H2CO3

In the first step, the solu(on is basic due to the forma(on of a salt where the basic part is
stronger than the acidic part (NaHCO3 ).So, in order to determine the equivalent
point of this reac(on Phenolphthalein is used. As the salt that forms due to the
neutraliza(on reac(on, produces more OH-, so the solu(on becomes a basic one and thus
it have a pH range above 7. We know that the working environment needed for
phenolphthalein is basic; thus phenolphthalein becomes the perfect indicator for
determining the end point of the first step of the reac(on.

In the second reac(on, NaCl and Carbonic Acid is formed. Because of the presence of
Carbonic Acid in the solu(on, it becomes acidic. So, ‘Methyl Orange’ (pH range 2.9-
4.6) is used as indicator to determine the equivalent point.