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Practical Physical Pharmaceutics 2012 PDF
Practical Physical Pharmaceutics 2012 PDF
Pr a ct ica l N ot e
Physica l
Ph a r m a ce u t ics
Done by:
Dr. Azza Ali Hasan
Assistant professor (Pharmaceutics)
First Year
Second Semester
Name:___________________________________
Academic Number:______________________
1
CONTENTS
Partition Coefficient
2
Physical Pharmaceutics (Practical)
Course Description :
Course Objectives :
3
Lab. 1.
Procedure:
2) Pour unknown liquid 1 into the graduated cylinder to the 25 ml. level.
Density= Mass/Volume
To calculate the mass for the liquid (you must subtract out the mass of the
graduated cylinder).
4
What is each liquid?
Using the table below it is now possible for you to determine what each
liquid is.
5
Lab. 2.
Procedure:
3. Using a small filter paper remove any attached humidity on the outside
of the apparatus.
4. Adjust the level of water to the upper mark and remove any suspended
drop.
5. Count the number of drops falling until the level of water reaches the
lower mark (undescended drop is not counted)
6. Repeat the procedure for unknown liquids after washing the apparatus
twice with the liquid to be measured.
7. Record your results in the following table, and represent the data
graphically.
6
Calculations & Results:
Water
Sample 1
Sample 2
Sample 3
where and are the surface tension of water and liquid. d1 and d2 are
the densities of water and liquid, respectively. n1 and n2 are the number of
drops of water and liquid.
7
Lab.3.
Procedure:
8
Lab.4.
Procedure:
9
Calculations and Results:
Distilled
water
Surfactant
solution
10
Lab.5.
Aim:
Procedure:
4. pipette out 5 ml of lower organic layer from the funnel into separate
flask using dry pipette.
11
End point Amount of benzoic acid dissolved
C aq S aq
12
Lab.5.
Procedure:
4. pipette out 5 ml of lower organic layer from the funnel into separate
flask using dry pipette.
Results:
13
Calculations & Results:
C aq S aq
14
Lab.6.
Procedure:
1. Take two stopper 250 ml iodine flasks A and B.
2. pipette out saturated solution of iodine in CCl4 and transfer 30 ml
iodine solution into flask A and 25 ml iodine solution into flask B.
3. Add 5 ml of pure CCl4 into flask B only to make the volumes same.
4. pour 120 ml of water each into the two flasks.
5. Put the stoppers and shake the flasks on a mechanized shaker for 15
minutes.
6. Allow it to stand for 10 min in separating funnel so that the layers
separate. While waiting, fill the burette with 0.01N Sodium Thiosulphate
solution.
7. From iodine flask A, pipette out 5 ml of organic layer into a conical
flask (organic layer should not be contaminated by the aqueous layer)
8. Titrate against 0.01N thiosulphate solution, without indicator till the
purple colour disappear.
9. Pipette out 20 ml of aqueous layer from the same bottle into the conical
flask, (adding starch at the beginning itself since the colour is light) and
titrate against 0.01N thiosulphate solution (till the blue colour
just disappears).
15
10. Repeat the two titrations for iodine flask B also. Calculate partition
coefficient for each flask.
Calculations & Results:
Partition coefficient of iodine between CCl4 and water = (1) _____ (2)
_____
Amount of Iodine dissolved
End point
Sample
(mls of 0.01 N In organic layer In aqueous layer
number
Na S2O3) E.P. F E.P. F
C org= mg/ C aq= mg/
5 20
ml ml
C aq S aq
16
Lab.7.
Aim:
pH meter
Beakers
Glass rod
Measuring cylinder
Procedure:
17
Stock solutions: A 0.2 M NaH2PO4 B 0.2 M Na2HPO4
A (ml) B (ml) pH
92.0 8.0 5.8
87.7 12.3 6.0
81.5 18.5 6.2
68.5 31.5 6.5
62.5 37.5 6.6
56.5 43.5 6.7
51.0 49.0 6.8
45.0 55.0 6.9
39.0 61.0 7.0
33.0 67.0 7.1
28.0 72.0 7.2
23.0 77.0 7.3
19.0 81.0 7.4
16.0 84.0 7.5
8.5 91.5 7.8
5.3 94.7 8.0
18
Lab.8.
19
Materials and apparatus:
pipetted into the lower bulb. The volume of water (15 mL) is chosen so
that the liquid can be conveniently sucked into the upper bulb leaving
2. Water is sucked up into the other bulb to a point about the mark above
the bulb.
3. Now it is released and stop clock is started when the meniscus crosses
the mark.
4. The clock is stopped when the mark below the bulb is passed.
used in calculations.
20
Calculations & Results:
Sample T1 T2 T3 Mean
Water
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
21
Lab.9.
Aim:
To follow the reaction by a titrimetric method and determination of the
first order rate constant by a graphical treatment of the data.
t is the time.
Procedure:
22
9. Cool to room temperature, pipette out 5 ml of solution into conical
flak containing 10 ml of ice cold water and repeat the titration.
10. The volume of NaoH consumed shall be taken as V .
11. Plot a graph of log (V -Vt) against time.
12. The slope gives the reaction rate constant.
Calculations & Results:
10
20
30
40
50
60
70
80
23
L o g c o n c e n tr a ti o n
Time
24
Slope = -k/2.303
Lab.10.
t is the time.
Procedure:
25
5. Similarly withdraw 10 ml samples at 5, 10, 15, 20, 25 and 30 min
intervals titrate the samples as earlier.
6. The titration values denote the amount of sodium hydroxide/ethyl
acetate remain unreacted i.e. "a-x"
7. Substituting these values in 2 nd order reaction.
8. Reaction gives the reaction rate constant or specific rate constant.
x
9. Plot a graph of Vs time "t" and calculate the slope.
a(a x)
EP Amount
(ml) Conc. decomposed
Time x 1 x
volume NaoH x K=
(min) a (a x) t a (a x)
of HCL (a-x)
added
10
15
20
25
30
26
Lab.11.
Procedure:
3. Shake the flasks at least 4 times, 2 min every 10 min, and then set
aside for 10 minutes to attain equilibrium.
4. Filter the contents of the flask separately through filter paper and
reject the first portion of the filtrate after washing the receiver with
it.
27
5. Titrate accurately measured portion (10 ml) of each filtrate with 0.5
N NaoH using phenolphthalein as indicator.
28
Normali Blank Experime Free (x/m) Log C Log (x/m)
ty E. P nt oxalic (mg/g
of (ml ) E. P C )
Oxalic (ml ) (mg/ml)
acid
0.1
0.2
0.3
0.4
0.5
29
Lab.12.
then, = tan -1 h / r
Lactose
Talc
starch
Funnel
30
Procedure:
31
Calculations & Results:
Angle of repose
powder Height (h) Radius (r)
( )
Sodium
chloride
(crystalline)
Acetyl salicylic
acid
starch
32
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