Lab

 Manuel    
Applied  Chemistry  III  CHEM-­‐05309      

List  of  Practical’s    

   
Ø  Measurement  of  water  hardness  with  EDTA  Titrations.    
Ø  Estimation  of  total  solids  in  water.    
Ø  Preparation  of  liquid  detergents.    
Ø  Extraction  of  capsicum  oil  (Soxhlet  Extractor)  
Ø  Extraction  of  clove  oil  from  cloves.    
Ø  Estimation  of  chloride  in  water.    
 

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                                                              Coverage  of  Contents  

Ø  Source  of  natural  essential  oil  

Ø  Market  value  of  essential  oil  
Ø  Various  methods  for  extraction  of  essential  oil  
Ø  History  (Soxhlet  Extractor)  
Ø  Objective  
Ø  Clove  oil  extraction  
Ø  BeneCits  of  clove  oil  
Ø  Assembly  of    Soxhlet  Extractor  
Ø  Theory  
Ø  Procedure  
Ø  Result  
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 History  of  Soxhlet  Extractor  
The   extraction   is   named   for   its   inventor,  
Franz   Ritter   von   Soxhlet   (1848–1926),   a  
German   chemist   who   worked   on   issues   of  
milk  chemistry.  He  developed  the  procedure,  
Cirst  described  in  1879,  as  a  way  to  separate  
the  fats  from  milk  solids.  ...  The  thimble  rests  
i n   t h e   b o t t o m   o f   t h e   b o d y   o f  
the   extractor   tube.   The   Soxhlet   Distillation  
Apparatus  is  typically  used  when  a  compound  
has   a   limited   solubility   or   when   the   impurity  
is  insoluble  in  a  solvent.  It  efCiciently  recycles  
a  small  amount  of  solvent  to  dissolve  a  large  
amount  of  material.  
 
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Extraction  of  Clove  oil  (Soxhlet  Extractor)  

OBJECTIVE  
 
1.  To  extract  fat  from  various  oil-­‐seeds  by  an  exhaustive  
extraction  using  a  Soxhlet  extractor.  
 
2.  To  determine  percent  of  fat  content  in  a  food  sample  by  
weight  in  a  sample.  
 
3.  To  study  the  function  of  extraction  process  by  Soxhlet  
extractor.  

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                                                                            Clove  oil  extraction  
 
Clove   (Syzygium   aromaticum)   is   an   aromatic   spice   used   by  
several   cultural   around   the   world.   It   is   also   known   as   clove  
bud,  it  has  been  cultivated  in  Europe  since  16  century  for  its  
number   of   uses.   Mostly   in   curried   dishes   and   spicy   fruitcake.  
Its  oil  is  very  beneCicial  for  health  
What  is  clove  bud  oil????  it  is  derived  from  clove  tree.  Clove  
tree   is   typically   found   in   low-­‐lying   areas   that   have   humid  
climate.  It  is  hard  plant  growing  well  in  poor  quality  soil  (but  
not   in   sandy   soil).   A   full-­‐grown   plant   may   reach   the   height   of  
10  m  or  12  m  with  tough  evergreen  leaves.  
Clove  oil  has  been  promoted  as  having  a  wide  range  of  health  
effect.  
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The   health   beneCits   of   clove   oil   can   be   attributed   to   its  
antimicrobial,  antifungal,  antiseptic,  antiviral,  aphrodisiac  and  
stimulating  properties.  The  oil  is  used  for  treating  a  variety  of  
health   disorders   including   toothaches,   indigestion,  
cough,   asthma,   headache,   stress   and   blood   impurities.   The  
most   important   and   common   use   of   clove   oil   is   in   dental   care.  
Several   toothpastes,   mouth   wash   and   oral   care   medications  
contain  clove  oil  as  an  important  ingredient.  
Clove  is  an  evergreen  tree,  which  produces  a  Clower  bud  that  
has  numerous  medicinal  properties.  It  is  often  referred  to  as  
clove  bud.  Clove  bud  has  a  shaft  and  a  head  and  hence  it  has  
the   Latin   name   clavus,   meaning   nail.   Clove   was   extensively  
used  in  ancient  Indian  and  Chinese  civilizations  and  it  spread  
to   other   parts   of   the   world,   including   Europe,   during   the  
seventh  and  eight  centuries.     9  
Even   now,   clove   is   used   in   several   Indian   and  
Chinese   dishes.Clove   is   rich   in   minerals   such  
a s   c a l c i u m ,   h y d r o c h l o r i c  
acid,   iron,   phosphorus,   sodium,   potassium,  
and  vitamin  A  and  vitamin  C.  

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 Apparatus  &  material  required  
Soxhlet  apparatus  
Cloves/  dried  and  grinded   Assembly  of  Soxhlet  apparatus  
Ethanol/n-­‐hexane,  
Stand  &  Clumps,  
Filter  paper/Cotton  
Boiling  chips,  Glass  
wool,  Soxhlet  glassware  
with  a  round-­‐bottomed  
 Clask,  Heating  mantle,  
 Concentrator    
(evaporation  apparatus)  
and  Analytical  balance.  
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Parts  of  Soxhlet  Extractor  

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Heating  mantle  with  round    

Bottom  Ylask   Sample  containing  apparatus  along    
With  siphon  
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Drying  &  grinding  of  Clove  /  

ready  for  pouring  in  thimble  

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Sample  containing  thimble  with  
Filter  paper  

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Condenser  with  inlet  &  outlet  point   Functional  inlet  &  outlet  Ylow  of  water  
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 Theory:    

The   term   “lipid”   refers   to   a   group   of   compounds   that   are  

insoluble   in   water,   but   show   variable   solubility   in   a   number   of  
organic   solvents.   The   lipid/oil   content   of   food   determined   by  
extraction   with   one   solvent   may   be   quite   different   from   the  
lipid   content   as   determined   with   another   solvent   of   different  
polarity.   Oil   content   is   determined   by   often   by   solvent  
extraction   methods,   but   it   is   also   can   be   determined   by   non-­‐
solvent   wet   extraction   methods   and   by   instrumental   methods  
that   rely   on   the   physical   and   chemical   properties   of   oil.   The  
method  of  choice  depends  on  a  variety  of  factors,  including  the  
nature   of   the   sample,   the   purpose   of   the   analysis   and  
instrumentation   available.   A   Soxhlet   extractor   is   a   piece   of  
laboratory  apparatus  invented  in  1879  by  Franz  von  Soxhlet.  It  
was   originally   designed   for   the   extraction   of   oils   from   a   solid  
material.     15  
However,  a  Soxhlet  extractor  is  not  limited  to  the  extraction  of  
lipids.  Typically,  a  Soxhlet  extraction  is  only  required  where  the  
desired  compound  has  a  limited  solubility  in  a  solvent,  and  the  
impurity   is   insoluble   in   that   solvent.   If   the   desired   compound  
has   a   signiAicant   solubility   in   a   solvent   then   a   simple   Ailtration  
can   be   used   to   separate   the   compound   from   them   insoluble  
substance.   This   experiment   so   uses   a   soxhlet   method   to  
determine  the  oil  contents  of  various  samples  especially  seeds.  
In   principle,   oil   is   extracted,   semi   continuously,   with   an   organic  
solvent.  Solvent  is  heated  and  volatized  then  is  condensed  above  
the  sample.  Solvent  drips  onto  the  sample  and  soaks  it  to  extract  
the   fat.   At   15-­‐20   min   interval,   the   solvent   is   siphoned   to   the  
heating   Clask,   to   start   the   process   again.   Fat   content   is  
measured  by  weight  loss  of  sample  or  weight  of  fat  removed.  
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Procedure  
1.  50g   of   the   ground   clove's   buds   was   weighed   and  
transferred  into  a  Cilter  paper  extraction  thimble,  thimble  
containing   the   sample   was   then   place   in   the   soxhlet  
extractor   Citted   at   the   lower   portion   with   a   Clask  
containing   300ml   of   n-­‐hexane   used   as   the   extraction  
solvent.    
2.  The   soxhlet   column   was   then   Citted   to   a   reClux   condenser  
and   the   set   up   was   placed   on   the   heating   mantle   as  
temperature  increase  steadily  until  n-­‐hexane  began  to  boil  
and   the   boiling   vapor   passes   through   the   condenser   and  
was  condensed,  
3.  Vapor  now  falls  back  on  the  porous  thimble  containing  the  
powdered   seed   sample,   n-­‐hexane   being   a   solvent  
dissolved  the  oil  content  of  the  seed  sample  leading  to  the  
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formation  of  homogenous  mixture  of  n-­‐hexane  and  

oil   which   was   collected   in   the   receiver   of   the  
soxhlet  extractor  set-­‐  up.  The  set-­‐up  was  heated,  for  
about  6  hours.    
 
Results  
 
%  age  of  extracted  oil  =    amount  of  oil  extracted  in  g    
                                                                                           amount  of  sample  taken  in  g    
 

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Capsicum  oil/Clove  extraction  by  Soxhlet  apparatus    

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Any Question??????