PRACTICAL PROTOCOL

Roll no- 23 Pages -

Aim :- To prepare validation protocol of a mixer and perform its validation of mixing
performance wit respect to low dose dr!g"
P!rpose :-
#$ Red!ction of %!alit& cost"
2$ Process validation"
3$ Ass!rance of %!alit& and safet&"
References :-
#$ Lac'man" L ( Li)erman *Te teor& and practice of ind!strial parmac& (+
,argese p!)lication page no" #-2-"
2$ Potdar A". *Parmace!tical /!alit& Ass!rance (+ 2--0 1irali p!)lication
page no" 2"32"
3$ 4aider 5"I *,alidation standard operating proced!re (+second edition page no
363-366"
Re%!irements :-
#$ Cemicals-
5r" 1o 1ame of Cemical /!antit& Ta'en
# Calci!m car)onate 7CaCo3$ #--gm
2 Potassi!m paramagnet 78m1o3$ #gm
3 Cr&stal violet
2$ 9lasswares -
5r " 1o 1ame Of 9lassware Capacit& /!antit&
# ,ials #- ml #-
2 5tirrer ----- -#
3 :ea'er #--ml -2
3 ,ol!metric flas' #--ml -#
6 ,ol!metric flas' #-ml -6
3$ Instr!ments ;
5r" 1o 1ame of Instr!ment .odel .a'e
# Colo!rimeter Potocal -<62 =%!ip-tronics
2 >o!)le cone )lender
Teor& :-
,alidation :-
A doc!mented programmed wic provides a ig degree of ass!rance tat specific
processes will consistenc& prod!ce a prod!ct meeting its predetermined specification
and %!alit& attri)!tes"
Importance of validation
#$ Red!ction of %!alit& cost"
2$ Process validation"
3$ Ass!rance of %!alit& and safet&"
.ixing :-
A process tat tends to res!lt in a randomi?ation of dissimilar particles ( witin a
s&stem or to p!t togeter in one mass or assem)lage wit more or less tro!g
diff!sion of te constit!ent elements among one anoter"
.ecanisms of mixing
#$ >iff!sion :- random action of individ!al particles in te mixer"
2$ Convection :- transfer of ad@acent particles gro!ps in te mixt!re "
3$ 5ear :- config!ration cange tro!g slip planes"
A$ =%!ipments !sed for mixing :- 7powder$
T!m)ler mixer
>o!)le cone )lender
Agitated powder mixer
Air mixer

:$ =%!ipments !sed for mixing :- 7li%!ids$
Propeller mixer
T!r)ine mixer
Paddle mixer
C$ =%!ipments !sed for mixing :- 7semisolid$
Triple roller mill
Agitator mixer
Planetar& mixer
>o!)le cone )lender :-
It is developed in an attempt to overcome some of te sortcoming of rotating
mixer" Te mixing of powder in do!)le cone )lender is d!e to t!m)ling and
searing action wit )lade " Te efficienc& of )lender depends mainl& on speed of
rotation "
Te rate of rotation so!ld )e optim!m wic depends !pon te si?e and sape of
t!m)ler as well as nat!re of material" Te common range is 3--#-- rpm"
Te material to )e )lended is loaded approximatel& 6--<-A of te total capacit&
of )lender " As te )lender rotates te material !ndergoes t!m)ling motion and mixes
te material"
Te do!)le cone )lender is an efficient design for mixing powder of difference
densities and is !sed mainl& for small %!antit& of powder"


Proced!re:- 7 Cali)ration c!rve of cr&stal violet $
#$ >issolve #-mg of cr&stal violet in # . 425O3 to prod!ce #--ml " 4eat te
sol!tion for 6-#-min 7!ntil )oil$"
2$ Cool te )ea'er sol!tion at room temp" and filter wit te elp of cotton pl!g
in f!nnel"
3$ Prepare dil!tion from te a)ove stoc' sol!tion #--mgBml to prod!ce conc"
#- CgBml and also prepare te 2(3(<(2(#- CgBml !sing #. 425O3"
3$ .eas!re te a)sor)ance on colorimeter"

O)servation Ta)le:-
Concentration A)sor)ance
2
3
<
2
#-
Proced!re :-
#$ Deig #--gm of CaCo3 and #gm of cr&stal violet and pass tem tro!g
sieve no <-"
2$ Load tose powder in do!)le cone )lender and note down te rpm of do!)le
cone )lender"
3$ Ta'e te samples from top( middle( and )ottom" >issolve tem in #-ml #.
425O3 in vials"
3$ Eilter it and meas!re te a)sor)ance !sing colorimeter"
6$ >etermine te conc" Fsing cali)ration c!rve and calc!late te std" deviation
of eac five interval( predict te optim!m time of mixing"
O)servation ta)le 7 I $ :-
5r" no Time Top .iddle :ottom
# 6
2 #-
3 #6
3 2-
6 26
< 3-
O)servation ta)le 7 II $ :-
5r" no Time Conc" Erom grap G dil" Eactor 7#--$ 5tandard
deviation Top .iddle :ottom mean
# 6
2 #-
3 #6
3 2-
6 26
< 3-
Res!lt :-
.ixing of cr&stal violet wit CaCO3 was carried o!t and validation parameter of
mixing were as )elow
5r" no Parameter .ixing metod 7 do!)le
cone )lender$
# i) CaCO3 #--gm
ii$ Cr&stal violet #gm
2 Optim!m mixing time
3 Conc" of optim!m time

5OP 1O -#23 =ffective date- ddBmmB&&
Approved )&- .r"a)c
Title - :lender 7 do!)le cone $
A!tor - 1ame B title B department
5ign date
Cec'ed )& - 1ame B title B department
5ign date
Approved )& - 1ame B title B department
5ign date
Revisions :-
5r" no 5ection Pages Initials B date
5OP 1O -#23 =ffective date- ddBmmB&&
Approved )&- .r"a)c
5!)@ect :- :lender 7 do!)le cone $
P!rpose:-
To descri)e te proced!re for validation of )lender to ens!re tat it meets installation(
operational( and performance %!alification re%!irements"
Responsi)ilit& :-
It is te responsi)ilit& of te prod!ction manager and tecnical services manager to
follow te proced!re" Te %!alit& ass!rance manager is responsi)le for 5OP
compliance"
Proced!re :-
#" ,erif& approved p!rcase order
2" ,erif& invoice
3" Cec' man!fact!rer and s!pplier
3" ,erif& model n!m)er and serial n!m)er
6" Cec' for an& p&sical damage
<" Confirm location and installation re%!irements per recommendation of
man!fact!rer"
0" ,erif& tat te re%!ired !tilities are availa)le
2" Installation sall )e cond!cted per instr!ction provided in te man!al"
H" =ns!re tat all relevant doc!mentation is received
i$ Fser man!al
ii$ .aintenance man!al
iii$ List of cange parts
iv$ =lectrical drawing
v$ .ecanical drawing