LABORATORY MANUAL
B.PHARM
SEMESTER – I
PHARMACEUTICAL INORGANIC CHEMISTRY
(BP110P)
Prepared by:
Ms. Mitali H. Jasani
Assistant professor (Pharmaceutical chemistry)
INDEX
Sr.
No
|
Title of experiments
|
|
1
|
Lab requirement & Introduction to
Pharma Chemistry
|
|
2
|
To perform limit test of chloride for given sample as per I.P 2010.
|
|
3
|
To perform limit test of chlorides in potassium permanganate sample
as per I.P 2010 (modified limit test of chloride)
|
|
4
|
To perform limit test of Sulphate for given sample as per I.P 2010..
|
|
5
|
To perform limit test of Sulphate in potassium permanganate sample as
per I.P 2010 (modified limit test of sulphate)
|
|
6
|
To perform limit test of Iron for given sample as per I.P 2010.
|
|
7
|
To perform limit test of heavy metals (lead) for given sample as per
I.P 2010.
|
|
8
|
To perform limit test of Arsenic for given sample as per I.P
2010.(demonstration)
|
|
9.
|
To determine swelling power of Bentonite
|
|
10.
|
To prepare boric acid from the given quantities of borax and
concentrated H2SO4.
|
|
11
|
To perform the identification test for ferrous sulphate
|
|
12
|
To perform the identification test for sodium bicarbonate
|
|
13
|
To perform the identification test for copper sulphate
|
|
14
|
To perform the identification test for magnesium hydroxide
|
|
15
|
To estimate neutralizing capacity of aluminium hydroxide gel I.P 2010
|
Practical: -1
Aim:
Lab
requirement & Introduction to Pharma Chemistry.
Requirement:
1.
Neat
& Clean Apron
2.
Journal
3.
Record
book
4.
Napkin
5.
Match
box
6.
Plastic
sheet
7.
Nicrome
wire
8.
Platinum
Loop
9.
Test
tubes (minimum-10)
10. Test tubes brush
11. Labels
12. Watch glass
13. Glass marker
14. Specula
15. Scientific
calculator
16. Soap/Detergent
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
|
Practical: -2
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 AgNO3 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 AgNO3 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
|
STANDARD
|
Ø Take 10ml of
test solution in nessler cylinder.
Ø Add 10ml
dil.HNO3.
Ø Dilute it upto
50ml with water.
Ø Add 1ml 0.1N
AgNO3 sol.
|
Ø Take 10ml of
Std. solution. in nessler cylinder.
Ø Add 10ml
dil.HNO3.
Ø Dilute it upto
50ml with water.
Ø 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
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
References:
Practical: -3
Aim: To perform
limit test of chloride in potassium permanganate sample as per I.P 2010
(modified limit test of chloride)
Requirement: Pair
of nessler cylinder, beaker, glass rod, AgNO3 sol., dil.HNO3, std.NaCl solution, KMnO4 sample
Principle:
Limit
test of Chloride is based upon simple reaction between AgNO3 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 AgNO3 to std. sol. of known amount of NaCl in presence
of dil. HNO3. As potassium permanganate solution is purple coloured
which interfere in the comparison of opalescence or turbidity, therefore the
aqueous solution must first be decolorize. So when potassium permanganate
solution is treated with ethanol (reducing agent)in presence of heat, redox
reaction takes place (i.e KMnO4 get reduced to MNO2(PPT). the
filtrate of the reactions colorless which is used for limit test for chlorides
Reaction
Cl-
+ AgNO3 → AgCl + NO3-
Procedure:
- Wash a pair
of nessler cylinder distilled water & dry it.
- Lable as
std. and test solution.
- Then
prepare solution as follows.
TEST
|
STANDARD
|
Ø Take 10ml of
test solution in nessler cylinder.
Ø Add 10ml
dil.HNO3.
Ø Dilute it upto 50ml with water.
Ø Add 1ml 0.1N
AgNO3 sol.
|
Ø Take 10ml of
Std. solution. in nessler cylinder.
Ø Add 10ml
dil.HNO3.
Ø Dilute it upto
50ml with water.
Ø 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 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 chloride in given sample is over/under the limit as per IP-2010,hence sample pass the limit test for chloride
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 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 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
References:
References:
Practical: -4
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 BaCl2 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
|
STANDARD
|
Ø Take 1ml of
25%W/V BaCl2 sol. in nessler cylinder.
Ø Add 1.5ml
ethanolic Sulphate std. solution.
Ø Mix well & allow it to stand for 1min. Ø Add 15ml test solution. Ø Add 0.15ml of 5M acetic acid.
Ø Make up the
vol. upto 50ml with distilled water.
|
Ø Take 1ml of
25%W/V BaCl2 sol. in nessler cylinder.
Ø Add 1.5ml
ethanolic Sulphate std. solution.
Ø Mix well & allow it to stand for 1min. Ø Add 15ml std. solution. Ø Add 0.15ml of 5M acetic acid.
Ø 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
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
References:
References:
Practical: -5
Aim: To perform
limit test of Sulphate in potassium permanganate sample as per I.P 2010
(modified limit test of sulphate)
Requirement: Pair of nessler
cylinder, beaker, glass rod, 25%BaCl2 sol., 5M CH3COOH,
solution of
Sulphate (20ppm), distilled water, KMnO4 sample
Principle:
Limit
test for Sulphate is based upon simple reaction between BaCl2 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. As potassium permanganate
solution is purple coloured which interfere in the comparison of opalescence or
turbidity, therefore the aqueous solution must first be decolorize. So when
potassium permanganate solution is treated with ethanol (reducing agent)in
presence of heat, redox reaction takes place (i.e KMnO4 get reduced to MNO2(PPT)).
the filtrate of the reactions colorless which is used for limit test for sulphate
Reaction
2KMnO4+3C2H5OH → 2 MnO2 +2 KOH +2 CH3CHO +
2H2O
Procedure:
- Wash a pair
of nessler cylinder distilled water & dry it.
- Lable as
std. and test solution.
- Then
prepare solution as follows.
TEST
|
STANDARD
|
Ø Take 1ml of
25%W/V BaCl2 sol. in nessler cylinder.
Ø Add 1.5ml
ethanolic Sulphate std. solution.
Ø Mix well & allow it to stand for 1min. Ø Add 15ml test solution. Ø Add 0.15ml of 5M acetic acid.
Ø Make up the
vol. upto 50ml with distilled water.
|
Ø Take 1ml of
25%W/V BaCl2 sol. in nessler cylinder.
Ø Add 1.5ml
ethanolic Sulphate std. solution.
Ø Mix well & allow it to stand for 1min. Ø Add 15ml std. solution. Ø Add 0.15ml of 5M acetic acid.
Ø Make up the
vol. upto 50ml with distilled water.
|
- · Stir both the solution. immediately by glass rod.
- · Allow both the cylinder to stand for 5 min. 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
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
References:
References:
Practical: -6
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)
Chemical
reaction:
Procedure:
- Wash a pair
of nessler cylinder distilled water & dry it.
- Lable as
std. and test solution.
- Then
prepare solution as follows.
TEST
|
STANDARD
|
Ø Take 2ml of
given sample of test solution and 20 ml of distilled water in nessler
cylinder
Ø Add 2ml 20 %
iron free citric acid
Ø Add 0.1 ml of
thioglycolic acid
Ø Make the
solution alkaline with iron free ammonia solution (about 15 ml)
Ø Dilute it with
50 ml with distilled water
|
Ø Take 2ml of
given sample of Std solution and 20 ml of distilled water in nessler cylinder
Ø Add 2ml 20 %
iron free citric acid
Ø Add 0.1 ml of
thioglycolic acid
Ø Make the
solution alkaline with iron free ammonia solution (about 15 ml)
Ø 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 is 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
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 is 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
The given solution PASS/FAIL with limit test for Iron as I.P. 2010
Practical: -7
Aim: To perform
limit test of heavy metals (lead) for given sample as per I.P 2010.
Requirement: Pair of Nessler
cylinder, beaker, glass rod, pipette, stand
Principle:
Limit
test of lead is based on the reaction of lead and diphenyl thiocabazone
(dithizone) in alkaline solution to form lead dithizone complex which is read
in color.
Dithizone
is green in color in chloroform and lead-dithizone complex is violet in color,
so the resulting color at the end of the process is red.
Chemical
reaction:
Procedure:
Test sample
|
Standard
compound
|
A known quantity of sample solution is
transferred in a separating funnel
|
A standard lead solution is prepared equivalent
to the amount of lead permitted in the sample under examination
|
Add 6ml of ammonium citrate
|
Add 6ml of ammonium citrate
|
Add 2 ml of potassium cyanide and 2 ml of
hydroxylamine hydrochloride
|
Add 2 ml of potassium cyanide and 2 ml of
hydroxylamine hydrochloride
|
Add 2 drops of phenol red
|
Add 2 drops of phenol red
|
Make solution alkaline by adding ammonia
solution.
|
Make solution alkaline by adding ammonia
solution.
|
Extract with 5 ml of dithizone until it becomes
green
|
Extract with 5 ml of dithizone until it becomes
green
|
Combine dithizone extracts are shaken for 30 mins
with 30 ml of nitric acid and the chloroform layer is discarded
|
Combine dithizone extracts are shaken for 30 mins
with 30 ml of nitric acid and the chloroform layer is discarded
|
To the acid solution add 5 ml of standard
dithizone solution
|
To the acid solution add 5 ml of standard
dithizone solution
|
Add 4 ml of ammonium cyanide
|
Add 4 ml of ammonium cyanide
|
Shake for 30 mins
|
Shake for 30 mins
|
Observe the color
|
Observe the color
|
Observation:
The intensity of the colour of complex, is depends on the amount of lead 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 colour of the test solution is more/less then the standard solution
Conclusion
The intensity of colour of the test solution is more/less then the standard solution.Therefore it is concluded that impurities of lead in given sample is over/under the limit as per IP-2010,hence sample pass the limit test for lead
Result
The given solution PASS/FAIL with limit test for lead as I.P. 2010
Practical: -8
Aim: To perform
limit test of Arsenic for given sample as per I.P 2010.(Demonstration)
Requirement: Pair
of nessler cylinder, gutzeit apparatus, beaker, glass rod, pipette, stand,
Principle:
Limit
test of Arsenic is based on the reaction of arsenic gas with hydrogen ion to
form yellow stain on mercuric chloride paper in presence of reducing agents
like potassium iodide. It is also called as Gutzeit test and requires special
apparatus.
Arsenic,
present as arsenic acid in the sample is reduced to arsenious acid by reducing
agents like potassium iodide, stannous acid, zinc, hydrochloric acid, etc.
Arsenious acid is further reduced to arsine (gas) by hydrogen and reacts with
mercuric chloride paper to give a yellow stain. The depth of yellow stain on
mercuric chloride paper will depend upon the quality of arsenic present in the
sample.
Chemical
reaction:
H3AsO4 +H2SnO2 →H3AsO3 +H2SnO3
Arsenicacid Arseniousacid
H3AsO3 +3H2 → AsH3 +3H2O
Arseniousacid Arsinegas
Arsenicacid Arseniousacid
H3AsO3 +3H2 → AsH3 +3H2O
Arseniousacid Arsinegas
GUTZEIT
APPARATUS
Procedure:
Test solution:
The test solution is prepared by dissolving specific amount in water and stannated HCl (arsenic free) and kept in a wide mouthed bottle.
To this solution 1 gm of KI, 5 ml of stannous chloride acid solution and 10 gm of zinc is added (all this reagents must be arsenic free)
Keep the solution aside for 40 min and stain obtained on mercuric chloride paper is compared with standard solution.
Standard solution:
A known quantity of dilute arsenic solution is kept in wide mouthed bottle and rest procedure is followed as described in test solution
The test solution is prepared by dissolving specific amount in water and stannated HCl (arsenic free) and kept in a wide mouthed bottle.
To this solution 1 gm of KI, 5 ml of stannous chloride acid solution and 10 gm of zinc is added (all this reagents must be arsenic free)
Keep the solution aside for 40 min and stain obtained on mercuric chloride paper is compared with standard solution.
Standard solution:
A known quantity of dilute arsenic solution is kept in wide mouthed bottle and rest procedure is followed as described in test solution
Observation
The
depth of the yellow stain depending upon the amount of arsenic present in the
sample, is compared with that of standard stain produced from a known amount of
arsenic. The depth of yellow stain on mercuric chloride paper will depend upon
the quality of arsenic present in the sample
Practical:
-9
Aim:
To determine swelling power of Bentonite
Requirements:
Chemicals &
Reagents: Bentonite, 1% sodium lauryl sulphate solution
Glassware: Measuring
cylinder, beaker
Description: Bentonite is a natural, colloidal, hydrated aluminium silicate that has been processed to remove grit and non-swelling components of the ore.A very fine, pale buff or cream-coloured to grayish-white powder, free or
almost free from gritty particles.
Category:
Pharmaceutical aid (suspending agent)
Procedure:
Add 2.0 g of bentonite in 20 portions at intervals of 2 minutes to 100 ml of a 1 per cent
w/v solution of sodium lauryl sulphate in a 100 ml graduated cylinder about 3
cm in diameter. Allow each portion to settle before adding the next and let it
stand for 2 hours.
Observation
table:
Sr. No
|
Time
|
Volume of
sediment (ml)
|
1
|
After 1 hour
|
|
2
|
After 2 hours
|
Result:
The
apparent volume of the sediment at the bottom of the cylinder is not less than
24 ml.
Conclusion:
The
given bentonite sample passes/fail the test for purity as per I.P 2010.
Reference:
Indian Pharmacopoeia 2010 vol II, page no 877.
Practical:
-10
Aim:
To prepare boric acid from the given quantities of borax and concentrated H2SO4.
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
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.
Reference:
Dr. G Devala Rao, Practical Pharmaceutical Inorganic Chemistry, Birla
publication, Ist edition page
no 55.
Practical:
-11
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.
Chemical
reactions:
The identification
reactions for ferrous sulphate are summarized as below:
A)
Identification test for Fe+2
Sr.
No
|
Test
|
Observation
|
Inference
|
1.
|
To
a small quantity of salt, add dilute H2SO4 and
phenanthroline
|
Red
colouration
|
Fe+2
may be present
|
2.
|
Add
ceric ammonium sulphate
|
Red
colour discharged
|
Fe+2
is confirmed
|
3.
|
Take
salt and add potassiun ferricyanide
|
Blue
precipitates observed
|
Fe+2
is confirmed
|
4.
|
Add
dilute HCl
|
Precipitates
are insolube
|
Fe+2
ion confirmed
|
5.
|
Take
salt and add potassiun ferrocyanide and add dilute HCl
|
White
precipitates are formed and rapidly becomes blue
|
Fe+2
may be present
|
6.
|
Add
dilute HCl
|
The
precipitates are insoluble
|
Fe+2
is confirmed
|
Result:
The given sample contains Fe+2 cations.
B)
Identification test for SO42-
Sr.
No
|
Test
|
Observation
|
Inference
|
1.
|
To
a small quantity of salt, add water with dilute HCl and BaCl2
|
White
precipitate
|
SO42-
may be present
|
2.
|
Take
salt and add lead acetate
|
White
precipitate
|
SO42-
may be present
|
3.
|
Add
CH3COONH4 with NaOH
|
Precipitate
dissolve
|
SO42-
ion confirmed
|
4.
|
Take
salt and add iodine solution
|
Suspension
of yellow colour is obtained
|
SO42-
may be present
|
5.
|
To
the above suspension, add SnCl2
and
boil the mixture
|
No
colour precipitate obtained
|
SO42-
ion confirmed
|
Result:
The given sample contains SO42- anions.
Practical:
-12
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:
The identification
reactions for sodium bicarbonate are summarized as below:
A)
Identification test for Na+
Sr.
No
|
Test
|
Observation
|
Inference
|
1.
|
Pyroantimonate
is added to prepared original solution
|
White
precipitates
|
Na+
is present
|
2.
|
Zinc
Uranyl acetate is added to prepared original solution
|
Yellow
precipitates
|
Na+
ion is confirmed
|
Result:
The given sample contains Na+ cations
Sr.
No
|
Test
|
Observation
|
Inference
|
1.
|
O.S.
+ dilute HCl
|
Effervesence
of CO2 gas that turns lime water milky
|
CO32-
is present
|
2.
|
O.S.
+ BaCl2 solution
|
White
precipitates soluble in dilute acid along with effervescence and also soluble
in excess of BaCl2
|
CO32-
is present
|
3.
|
O.S.
+ AgNO3
|
White
precipitates that turn yellow on adding an excess of the reagent and the
precipitates dissolved rapidly in dilute HNO3 or ammonia
|
CO32-
ion is confirmed
|
Result:
The given sample contains CO32- anions.
Practical:
-13
Aim:
To perform the identification test for copper sulphate
Reference:
H.G
Raval, Practicals in Inorganic and
Analytical Chemistry, Nirav and Roopal Prakasan, Ist edition, Page
no. 22.
Requirements:
Chemicals &
Reagents: Copper sulphate powder, potassium ferrocyanide, H2S water,
dilute NaOH, dilute NH4OH, potassium iodide solution, barium
chloride solution, lead acetate, ammonium acetate, dilute NaOH, iodine
solution, strontium chloride.
Glassware: Test tube,
beaker, funnel watch glass, spatula
Chemical
formula: CuSO4.5H2O
Theory:
Cupric sulfate is
a white or off-white solid. The anhydrous salt is colourless but the
hydrated salt is blue in colour. It readily dissolves in water but is insoluble
in alcohol. The pentahydrate (CuSO4·5H2O),
the most commonly encountered salt, is bright blue.
Uses: It is a potent emetic
and is used as an antidote for poisoning by phosphorus.
Reactions:
The identification
reactions for copper sulphate are summarized as below:
A)
Identification test for Cu+2
Sr.
No
|
Test
|
Observation
|
Inference
|
1.
|
O.S.
+ K4Fe(CN)6
|
Reddish
brown ppt obtained
|
Cu+2
is present
|
2.
|
O.S.
+ H2S
|
Black
precipitates
|
Cu+2
is present
|
3.
|
O.S.
+ NaOH
|
Blue
precipitates
|
Cu+2
is present
|
5.
|
O.S.
+ NH4OH
|
Bluish
green precipitate which dissolves in excess ammonia
|
Cu+2
ion is confirmed
|
6.
|
O.S.
+ KI
|
Greenish
white or brown precipitates
|
Cu+2
ion is confirmed
|
Result:
The given sample contains Cu+2 cations
B)
Identification test for SO42-
Sr.
No
|
Test
|
Observation
|
Inference
|
1.
|
To
a small quantity of salt, add water with dilute HCl and BaCl2
|
White
precipitate
|
SO42-
may be present
|
2.
|
Take
salt and add lead acetate
|
White
precipitate
|
SO42-
may be present
|
3.
|
Add
CH3COONH4 with NaOH
|
Precipitate
dissolve
|
SO42-
ion confirmed
|
4.
|
Take
salt and add iodine solution
|
Suspension
of yellow colour is obtained
|
SO42-
may be present
|
5.
|
To
the above suspension, add SnCl2
and
boil the mixture
|
No
colour precipitate obtained
|
SO42-
ion confirmed
|
Result:
The given sample contains SO42- anions
Practical:
-14
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:
A)
Identification test for Mg2+
Sr.
No
|
Test
|
Observation
|
Inference
|
1.
|
Take
15 mg of substance being examined. Add 2 ml of H2O and 1 ml of
dilute NH3 solution.
|
A
white precipitate is formed
|
Mg2+
may be present
|
2.
|
To
the above solution, add 1 ml of 2 M NH4Cl
|
Precipitates
redissolves
|
Mg2+
confirmed
|
3.
|
Add
1 ml of 0.25 M of Na2HPO4
|
A
white crystalline ppt is formed
|
Result:
The given sample contains Mg2+ cations
B)
Identification test for OH-
Sr.
No
|
Test
|
Observation
|
Inference
|
1.
|
Perform
litmus paper test for O.S
|
Red
litmus paper turns to blue
|
OH-
may be present
|
2.
|
O.S.
+ HgCl2 solution
|
Yellow
precipitates
|
OH-
is confirmed
|
Result:
The given sample contains OH- anions
Practical: -15
Aim: To estimate neutralizing
capacity of aluminium hydroxide gel I.P 2010
Synonym:
Aluminium hydroxide suspension, Aluminium hydroxide mixture
Requirements:
Chemicals
& Reagents: Dried aluminium hydroxide, 0.1 M hydrochloric acid, 0.1 M
sodium hydroxide
Glassware:
Burette, beaker, funnel, glass rod, conical flask, measuring cylinder.
Description:
A white, viscous suspension translucent in thin layers; small amounts of clear
liquid may separate on standing. Aluminium Hydroxide Gel is an aqueous suspension
of hydrated aluminium oxide together with varying quantities of basic aluminium
carbonate and bicarbonate. It may contain Glycerin, Sorbitol, Sucrose or
Saccharin as sweetening agents and peppermint oil or other suitable flavours.
It may also contain suitable antimicrobial agents.Aluminium Hydroxide Gel
contains not less than 3.5 per cent and not more than 4.4 percent w/w of Al2O3
Category:
Antacid
Procedure:
Disperse 5.0 g in 100 ml of water, heat to 37
̊C,
add 100.0 ml of 0.1 M hydrochloric acid previously heated to 37 ̊C and stir continuously, maintaining the
temperature at 37 ̊C; the pH of the
solution, at 37 ̊C, after 10, 15 and 20
minutes, is not less than 1.8, 2.3 and 3.0 respectively and at no time is more
than 4.5. Add 10.0 ml of 0.1 M hydrochloric acid previously heated to 37 ̊C, stir continuously for 1 hour
maintaining the temperature at 37 ̊C and titrate with 0.1
M sodium hydroxide to pH 3.5.
Observation
Calculation
Result
The
neutralizing capacity of aluminium hydroxide gel was found to be ………………
Reference: Indian
Pharmacopoeia 2010 vol II, page no 788.
The
International Pharmacopoeia - Sixth Edition, 2016
