EXPERIMENT NO 01

AIM: To study the different glassware used in pharmaceutical laboratory.

Reference: Dr. Rao Devala G, “ Practical Pharmaceutical Analysis”, Birla

Publication pvt ltd, 5th edition 2017-18, pg no 9-12.

Requirements: All glassware present in laboratory

Theory: laboratory glassware refers to a variety of equipments in scientific work

traditionally made of glass.

General Laboratory rules:

1. Always wear apron before entering in lab
2. Keep silence during working
3. Keep working place neat & clean
4. Reagent bottle must be kept on same place after use
5. Throw all rubbish in dust bin
6. Safety process must be followed
7. Don’t waste gas, chemical & water.
8. Don’t leave laboratory without permission of lab instructor
9. Always follows the instruction carefully, does not divert it.

Introduction of apparatus used in laboratory:

Sr no. Name Use

1. Burette Titration

2. Volumetric flask To measure the volume of solution

3. Iodine flask To prepare solution ,it air tight

4. Pipette For accurate measurement of volume

5. Beaker For putting the sample

6. Measuring Cylinder For appropriate measurement of volume

7. Nesseler cylinder To perform limit test

8. Ostwald viscometer For measurement of viscosity of solution

9. Stalagmometer For measurement of surface tension of liquid

10. Wire gauze As a support during heating

11. Pair of tongs For holding the hot material

12. Glass rod To stir the solution

Result: The different types of glassware were ………..

Viva Voce

Q1. Which type of glass type mostly used for preparing pharmaceutical glassware?

Q2. What is soda lime glass?

Q.3 Name the different size of seives used in laboratory?

Q.4 How you can calibrate Volumetric flask?

Q5. What is stalagmometer?

 EXPERIMENT 02

Aim: To perform limit test of chloride for given sample as per I.P 2010

Requirement: Pair of nessler cylinder, beaker, glass rod, AgNO3 sol.,

dil.HNO3, std. NaCl solution.

Principle:
Limit test of Chloride is based upon simple reaction between AgNO 3 and soluble
chloride to obtain AgCl which is insoluble in dil.HNO3 which makes the solution
turbid. The extent of turbidity depends upon the amount of chloride present in
substance and compared with std. turbidity produced by addition of AgNO 3 to std.
sol. of known amount of NaCl in presence of dil. HNO3.

Cl- + AgNO3 → AgCl + NO3-

NaCl + AgNO3 → AgCl + NaNO3
Procedure:
 Wash a pair of nessler cylinder distilled water & dry it.
 Lable as std. and test solution.
 Then prepare solution as follows.

TEST
Take 10ml of test solution in
nessler cylinder.
Add 10ml dil.HNO3.
Dilute it upto 50ml with
water.
Add 1ml 0.1N AgNO3 sol.
STANDARD
Take 10ml of Std. solution. in
nessler cylinder.
Add 10ml dil.HNO3.
Dilute it upto 50ml with
water.
Add 1ml 0.1N AgNO3 sol.

 Stir both the solution immediately by glass rod.

 Allow both the cylinder to stand for 5min
 Compare turbidity of test & std. sol. by viewing in front of dark
background.
Observation:
The intensity of the turbidity is depends on the amount of chloride present in the
solution. The turbidity developed in test and standard solution is compared by
viewing over dark background.The extent of turbidity of the test solution
is more/less than the standard solution

Conclusion
The extent of turbidity of the test solution is more/less than the
standard solution.therefore it is concluded that impurities of chloride in given
sample is over/under the limit as per IP-2010,hence sample pass the limit test for
chloride

Result
The given solution PASS/FAIL with limit test for chloride as I.P. 2010
 EXPERIMENT 03

Aim: To perform limit test of Sulphate for given sample as per I.P 2010.

Requirement: Pair of nessler cylinder, beaker, glass rod, 25%BaCl2 sol., 5M

CH3COOH,
solution of Sulphate (20ppm), distilled water.
Principle:
Limit test for Sulphate is based upon simple reaction between BaCl 2 and dil.HCl or
CH3COOH. This results the formation of BaSO4. The extent of turbidity of test
solution compared with std. turbidity which depends upon amount of Sulphate
impurity.

Procedure:
 Wash a pair of nessler cylinder distilled water & dry it.
 Lable as std. and test solution.
 Then prepare solution as follows.

TEST
Take 1ml of 25%W/V BaCl2sol. in
nessler cylinder.
Add 1.5ml ethanolic Sulphate std.
solution.
Mix well & allow it to stand
for 1min.
Add 15ml test solution.
Add 0.15ml of 5M acetic acid.
Make up the vol. upto 50ml with
distilled water.
STANDARD
Take 1ml of 25%W/V BaCl2sol. in
nessler cylinder.
Add 1.5ml ethanolic Sulphate std.
solution.
Mix well & allow it to stand for
1min.
Add 15ml std. solution.
Add 0.15ml of 5M acetic acid.
Make up the vol. upto 50ml with
distilled water.

 Stir both the solution immediately by glass rod.

 Allow both the cylinder to stand for 5min. protect from sunlight
 Compare turbidity of test & std. sol. by viewing in front of dark
background
Observation:
The intensity of the turbidity is depends on the amount of sulfate present in the
solution. The turbidity developed in test and standard solution is compared by
viewing over dark background.The extent of turbidity of the test solution
is more/less then the standard solution.

Conclusion
The extent of turbidity of the test solution is more/less then the
standard solution.therefore it is concluded that impurities of sulfate in given
sample is over/under the limit as per IP-2010,hence sample pass the limit test for
sulfate

Result The given solution PASS/FAIL with limit test for sulfate as I.P. 2010
.
 EXPERIMENT 04
Aim: To perform the identification test for ferrous sulphate

Reference: Dr. N. Sharma, Practical Inorganic Pharmaceutical Chemistry And

Viva Voce, Birla Publications Pvt. Ltd., Ist edition, Page no. 83-84.

Requirements:
Chemicals & Reagents: Ferrous sulphate crystals, dilute H2SO4, phenanthroline,
ceric ammonium sulphate, potassiun ferricyanide, dilute HCl, potassiun
ferrocyanide, barium chloride, lead acetate, ammonium acetate, dilute NaOH,
iodine solution, strontium chloride.
Glassware: Test tube, beaker, funnel watch glass, spatula

Chemical Formula: FeSO4.7H2O

Theory: Ferrous sulfate occurs as a crystalline bluish green powder. It has a

tendency to rapidly oxidize on exposure to moist air. It is odorless and is
characterized through its metallic taste (styptic) taste. It is soluble in water but
insoluble in alcohol.
Use: It is used as an important hematinic agent in various iron formulations for
treatment of anemia.
The identification reactions for ferrous sulphate are summarized as below:
A) Identification test for Fe+2

Sr.
Test Observation Inference
No
To a small quantity of salt, add
Fe+2 may be
1. dilute H2SO4 and Red colouration
present
phenanthroline
Red colour
2. Add ceric ammonium sulphate Fe+2 is confirmed
discharged
Take salt and add potassiun Blue precipitates
3. Fe+2 is confirmed
ferricyanide observed
Precipitates are
4. Add dilute HCl Fe+2 ion confirmed
insolube
White precipitates
Take salt and add potassiun Fe+2 may be
5. are formed and
ferrocyanide and add dilute HCl present
rapidly becomes
 blue
The precipitates
6. Add dilute HCl Fe+2 is confirmed
are insoluble

Result: The given sample contains Fe+2 cations.

B) Identification test for SO42-

Sr. Test Observation Inference

No
1. To a small quantity of salt, add White precipitate SO42- may be
water with dilute HCl and present
BaCl2
2. Take salt and add lead acetate White precipitate SO42- may be
present
3. Add CH3COONH4 with NaOH Precipitate SO42- ion
dissolve confirmed
4. Take salt and add iodine Suspension of SO42- may be
solution yellow colour is present
obtained
5. To the above suspension, add No colour SO42- ion
SnCl2 precipitate confirmed
and boil the mixture obtained

Result: The given sample contains SO42- anions.

 EXPERIMENT 05

Aim: To perform the identification test for sodium bicarbonate

Reference: H.G Raval, Practicals in Inorganic and Analytical Chemistry, Nirav

and Roopal Prakasan, Ist edition, Page no. 39.

Requirements:
Chemicals & Reagents: Sodium bicarbonate powder, pyroantimonate, Zinc uranyl
acetate, dilute HCl, BaCl2 solution, freshly prepared silver nitrate solution.
Glassware: Test tube, beaker, funnel watch glass, spatula

Chemical formula: NaHCO3

Theory: Sodium bicarbonate is a white solid crystalline compound composed of

sodium ions and bicarbonate ions. It has a slightly salty, alkaline taste resembling
that of washing soda (sodium carbonate). Sodium bicarbonate is also known as
baking soda.
Use: Sodium bicarbonate is used to relieve heartburn, sour stomach, or acid
indigestion by neutralizing excess stomach acid.
Category: Antacid
Reactions:
2 Na+ + K2H2Sb2O7 → Na2H2Sb2O7 (white precipitate) + 2K+
Na2CO3 + BaCl2 → BaCO3 (white precipitates) + 2NaCl
Na2CO3 + 2HCl → 2NaCl + H2O + CO2
Na2CO3 + 2AgNO3 → Ag2CO3 (white precipitate) + 2NaNO3
The identification reactions for sodium bicarbonate are summarized as below:
A) Identification test for Na+

Sr.
Test Observation Inference
No
Pyroantimonate is added to
1. White precipitates Na+ is present
prepared original solution
Zinc Uranyl acetate is added to Yellow
2. Na+ ion is
prepared original solution precipitates

Result: The given sample contains Na+ cations

Sr.
Test Observation Inference
No
Effervesence of
CO2 gas that CO32- is present
1. O.S. + dilute HCl
turns lime water
milky
White
precipitates
soluble in dilute
acid along with CO32- is present
2. O.S. + BaCl2 solution
effervescence
and also soluble
in excess of
BaCl2
White
precipitates that
turn yellow on
adding an excess
of the reagent CO32- ion is
3. O.S. + AgNO3
and the confirmed
precipitates
dissolved rapidly
in dilute HNO3 or
ammonia

Result: The given sample contains CO32- anions.

 EXPERIMENT 06

Aim: To perform the identification test for magnesium hydroxide

Reference: H.G Raval, Practicals in Inorganic and Analytical Chemistry, Nirav

and Roopal Prakasan, Ist edition, Page no. 22.

Requirements:
Chemicals & Reagents: Magnesium hydroxide powder, Ammonia solution,
ammonium chloride solution, sodium hydrogen phosphate, litmus paper,
HgCl2 solution
Glassware: Test tube, beaker, funnel watch glass, spatula
Chemical formula: Mg(OH) 2
Theory: Magnesium hydroxide is a white solid with low solubility in
water Magnesium is important for many systems in the body especially the
muscles and nerves. Magnesium hydroxide is used as a laxative to relieve
occasional constipation (irregularity) and as an antacid to relieve indigestion, sour
stomach, and heartburn.
Uses: Magnesium hydroxide is a common component of antacids, such as milk of
magnesia, as well as laxatives.
Reactions:
Mg2+ + Na2HPO4 + NH3 Mg (NH4) PO4 (white part)
2+
A) Identification test for Mg

Sr. Test Observation Inference

No
1. Take 15 mg of substance being A white precipitate Mg2+ may be
examined. Add 2 ml of H2O is formed present
and 1 ml of dilute NH3solution.
2. To the above solution, add 1 ml Precipitates
of 2 M NH4Cl redissolves Mg2+ confirmed
3. Add 1 ml of 0.25 M of A white crystalline
Na2HPO4 ppt is formed

Result: The given sample contains Mg2+ cations

B) Identification test for OH-

Sr. Test Observation Inference
 No
1. Perform litmus paper test for Red litmus paper OH- may be
O.S turns to blue present
2. O.S. + HgCl2 solution Yellow OH- is confirmed
precipitates

Result: The given sample contains OH- anions

 EXPERIMENT 07
Aim: To prepare boric acid from the given quantities of borax and
concentrated H2SO4.

Reference: Dr. G Devala Rao, Practical Pharmaceutical Inorganic Chemistry,

Birla publication, Ist edition page no 55.

Requirements:
Chemicals & Reagents: Borax, concentrated H2SO4, distill water.
Glassware: Beakers, Measuring jar, Glass rod, funnel.
Principle: Sodiun tetraborate (borax) on reaction with acid like HCl/H2SO4 gives
insoluble boric acid. It precipitates as white precipitate. It is collected washed free
from acid dried and weighed. The reaction involved are as follows:

Na2B4O7 + H2SO4 + 5H2O → Na2SO4 + 4H3BO3

Procedure: Dissolve 30 gm of borax in 50 ml of distilled water. Boil the solution.

Add a mixture of concentrated H2SO4 (6 ml) amd water (60 ml) to the boiled
solution slowly with constant stirring. Hot liquid is filtered and kept aside for
crystallization. The boric acid is filtered washed with water to remove soluble
sulphates. Dry boric acid at room temperature and weigh. Report the yield of boric
acid in grams.
Uses: boric acid is an example of topical agent (antiseptic).

Result: The yield of boric acid is obtained as ___gm.

 EXPERIMENT 08
Aim: To perform limit test of Iron for given sample as per I.P 2010.

Requirement: Pair of nessler cylinder, beaker, glass rod, pipette, stand

Principle:
Limit test for iron is based upon simple reaction between thioglycolic acid and iron
in the presence of citric acid and Ammonical alkaline medium.
This results the formation of purple coloured ferrous salt of thioglycolic acid
(ferrous thioglycolate complex)

Procedure:
 Wash a pair of nessler cylinder distilled water & dry it.
 Lable as std. and test solution.
 Then prepare solution as follows.

TEST STANDARD

Take 2ml of given sample of test
solution and 20 ml of distilled water
in nessler cylinder
Add 2ml 20 % iron free citric acid
Add 0.1 ml of thioglycolic acid
Make the solution alkaline with iron
free ammonia solution (about 15 ml)
Dilute it with 50 ml with distilled
water
Take 2ml of given sample of Std
solution and 20 ml of distilled water
in nessler cylinder
Add 2ml 20 % iron free citric acid
Add 0.1 ml of thioglycolic acid
Make the solution alkaline with iron
free ammonia solution (about 15 ml)
Dilute it with 50 ml with distilled
water

 Stir both the solution immediately by glass rod.

 Allow both the cylinder to stand for 5min
 Compare intensity of colour of both the solution

Observation:
The intensity of the colour of complex, is depends on the amount of iron present in
the solution.The intensity developed in test and standard solution is compared by
viewing over a white tile through the solution The intensity of pale pink
to purple colour of the test solution more/less then the standard solution

Conclusion
The intensity of pale pink to purple colour of the test solution is more/less then the
standard solution. Therefore it is concluded that impurities of iron in given sample
is over/under the limit as per IP-2010,hence sample pass the limit test for iron

Result
The given solution PASS/FAIL with limit test for Iron as I.P. 2010
 EXPERIMENT 09

Aim: To prepare and standardize 0.1 N Hcl.

Reference: Baghel Singh Dr. Uttam, Kabra Ruchika, Kabra Atul, “Pharmaceutical
Inorganic Chemistry”, S. Vikas and compamy , Scecond edition 2018, pg no 164-
168.

Requirement: Conical Flask, Burette, beaker, measuring cylinder, funnel,

volumetric flask.

Theory: Volumetric analysis is a widely-used quantitative analytical method. As

the name implies, this method involves the measurement of volume of a solution of
known concentration which is used to determine the concentration of the analyte.
Basic principles of volumetric analysis the solution to be analyzed contain an
unknown amount of chemicals. The reagent of unknown concentration reacts with
a chemical of an unknown amount in the presence of an indicator (mostly
phenolphthalein) to show the end-point. It’s the point indicating the completion of
the reaction. The volumes are measured by titration which completes the reaction
between the solution and reagent. The volume and concentration of reagent which
are used in the titration show the amount of reagent and solution. The amount of
unknown chemical in the specific volume of solution is determined by the mole
fraction of the equation.

Normality: Normality (N) is defined as the number of mole equivalents per liter of
solution:
normality = number of mole equivalents/1 L of solution
Normality in relation of titration
N1V1=N2V2

Procedure:
Preperation of 0.1 N Hcl
4.3 ml of Hcl was taken and the volume was made upto 500ml with distilled
water.

For standardization
1) 0.08gm of NaOH was taken and dissolve in 200ml of distilled water.
2) The burette is rinse before performing experiment then it was filled
with Hcl solution.
 3) A conical flask was placed beneath the burette.
4) To it add 10ml of NaOH solution and 2-3 drop of methyl orange
indicator was added.
5) Take 3ml of reading after titration clean the glass ware

Result: The Normality of 0.1 N HCl is ……….