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1.2        Methods of
a Describe methods of separations analysis
        purification and and purification          for the
) components of the following types of mixtures:
   (i) solid-solid
   (ii) solid-liquid
   (iii) liquid-liquid (miscible and immiscible)
                                     Done by: Chew Yun Jin (3)
                                               3H/2011
Techniques to be covered for separations and purification include:
(i) Use of suitable solvent, filtration and crystallization
       or evaporation
(ii) Sublimation
(iii) Distillation and fractional distillation
(iv) Use of a separating funnel
(v) Paper chromatography
Separating a Solid
from Solid. . .
 Filtration

I   t    i s    u   s   e d    t   o
s   e   p a r   a   t   e o    n   e
s   o   l u b   l   e    s o   l   i d a n d
a   n   o t h   e   r    s o   l   i d .
Ho w d o we u s e f i l t r a t i o n t o
s e p a r a t e t wo s o l i d s ?

A    mi x t u r e o f t w o s o l i d s c a n     a l s o
b   e s e p a r a t e d b y f i l t r a t i o n   i f o n e
o   f t h e m a r e s o l u b l e i n a s o l     v e n t
b   u t t h e o t h e r i s n o t . Fo r
e   x a mp l e , a mi x t u r e o f s a l t a     n d
s   a n d c a n b e s e p a r a t e d b y
f   i l t r a t i o n u s i n g wa t e r a s t    h e
E x p e r i me n t        3
T o s e p a r a t e a mi x t u r e o f c o mmo n t a b l e s a l t
a n d s a n d
Pr o c e d u r e :
1) P o u r s o m e d i s t i l l e d w a t e r i n t o t h e
   mi x t u r e o f c o mmo n t a b l e s a l t a n d s a n d .
   S t i r a n d w a r m t h e mi x t u r e .
2) P o u r t h e w a r m m i x t u r e i n t o a f i l t e r
   f u n n e l l i n e d wi t h f i l t e r p a p e r . Co l l e c t
   t h e f i l t r a t e i n a c o n i c a l f l a s k (F i g . 3.14).
3) Wa s h t h e r e s i d u e w i t h a l i t t l e d i s t i l l e d
   w a t e r t o r e mo v e a l l t h e s a l t s o l u t i o n
   f r o m i t . Th e r e s i d u e i s s a n d .
4) P o u r t h e f i l t r a t e i n t o a n e v a p o r a t i n g
   d i s h a n d e v a p o r a t e t h e f i l t r a t e t o
   d r y n e s s (F i g . 3.15). T h e w h i t e s o l i d l e f t i n
   t h e e v a p o r a t i n g d i s h i s s a l t .
A n o t h e r E x a mp l e :
To s e p a r a t e s a l t a n d
c h a l k p o wd e r


-D i s s o l v e t h e   mi x t u r e u s i n g
d i s t i l l e d wa t   e r .
-T h e s a l t w i l l    d i s s o l v e i n
wa t e r wh i l e
 t h e s a n d wi l l     r e ma i n i n t h e
b e a k e r .
-T h e f i l t e r p a   p e r   o n l y a l l o ws
t h e
 s o l u t i o n t o p   a s s t h r o u g h .
Cr y s t a
    l l i z a t
-C o l l e c t t h e
    i t o an e a n d p l
f i l   r   t              a c e
i t
 i n t o a n
e v a p o r a t i n g d i s h .
-E v a p o r a t e t h e
wa t e r / s o l v e n t
u n t i l
 t h e s o l u t i o n i s
s a t u r a t e d . (D o n o t
 h e a t t o d r y n e s s )
-C o o l t h e s o l u t i o n
a n d c r y s t a l s wi l l
Separating a Solid
from a Liquid. . .
Decanting
The simplest way to separate the water from the
pebbles is to just pour the water away. This
method is called decanting (Fig 3.10) We use
decanting to separate a dense, insoluble solid
from a liquid. Decanting is carried out everyday
during many activities. For example during
cooking, water is poured off various cooked foods
by decanting.
Filtration
To separate sand from water, we use a
method known as filtration. In general,
we use filtration to separate small solid
particles from liquid. Examples of small
solid particles include sand, clay, dust
particles and precipitates (small solid
particles produced in a liquid by chemical
reactions)
How can we remove a precipitate from
a reaction mixture by filtration?
A white precipitate of lead (II) sulfate is
produced when we add sodium sulfate
A    s o l i d     c a     n b e s e p a r a t e      d f      r   o   m a l i q u i     d b y
f   i l t r a t    i o     n b e c a u s e t h e       f i     l   t   e r p a p e r     a c t s
a   s a s i e      v e     . A l i q u i d c a n       p a     s   s    t h r o u g h   t h e
p   o r e s (s     ma      l l h o l e s ) o f t      h e      f   i   l t e r p a p    e r b u t
a    s o l i d     c a     n n o t d o s o .

Up    o   n f i    l   t   r a t i o n , t h   e s o l    i    d    t h a t r e ma i n s o n
t h   e    f i l   t   e   r p a p e r i s      c a l l    e   d    t h e r e s i due . Th e
l i   q   u i d    o   r    s o l u t i o n    t h a t     p   a   s s e s t h r o u g h t h e
f i   l   t e r    p   a   p e r i s c a l     l e d t     h   e    f i l t r a t e .
Evaporation to Dryness
and Crystallization
When a solid is insoluble in water, the easiest way to separate it from a liquid is by filtration.
However, many substances, like common salt, dissolve in water to form solutions. To
separate such substances, we evaporate water from the solution. This separation technique
is called evaporation to dryness. Fro example, when we evaporate salt solution to
dryness, we recover solid salt. This method can be used to recover salt from seawater.

However, many substances decompose when they are heated strongly. For example, sugar
will decompose to give water and carbon when it is heated strongly. Most crystals, such as
copper (II) sulfate crystals, give off water to become powders when heated. For such
substances, evaporation to dryness is nota good method of purification. Also, when all the
water is removed during evaporation, any soluble impurities present will be left on the
crystals.
The best method of obtaining a pure solid sample solution is called crystallization.

  How do we purify by crystallization?
  In crystallization, water is removed by heating the solution. Heating is stopped at the stage
  when a hot saturated solution is formed. If the resulting solution is allowed to cool to room
  temperature, the dissolved solid will be formed as pure crystals.

  How do we test for a saturated solution?
  A clean glass rod can be used to test whether a solution is saturated. It is dipped into the
  solution and removed. There will be a small amount of solution on the rod. If small crystals
  form on the rod as the solution cools, the solution is saturated. The solution is at its
  saturation point or crystallization point.
Example: Obtaining copper (II) sulfate crystals from copper (II) sulfate solution
Flowchart below shows the steps involved.
                                   Heat until the solution
      Copper (II) sulfate          is saturated                Saturated copper (II)
          solution                                               sulfate solution
                                                     Allow solution to cool
                                                                 Copper (II) sulfate
      Copper (II) sulfate          Filter the mixture            crystals + solution
          solution                                               (contains soluble
                                                                     impurities)
Websites for extra
information :        & http://www.youtube.com/watch?v=aFONmzLQJSY
Done by:
                          Chew Yun Jin (3)
                          3H/2011



1)Chemistry Matters
   (Marshall Cavendish)
  textbook
2) www.chemcompass.pbwo
   rks.com
3) www.google.com

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Experimental chemistry- part 1

  • 1. 1.2 Methods of a Describe methods of separations analysis purification and and purification for the ) components of the following types of mixtures: (i) solid-solid (ii) solid-liquid (iii) liquid-liquid (miscible and immiscible) Done by: Chew Yun Jin (3) 3H/2011
  • 2. Techniques to be covered for separations and purification include: (i) Use of suitable solvent, filtration and crystallization or evaporation (ii) Sublimation (iii) Distillation and fractional distillation (iv) Use of a separating funnel (v) Paper chromatography
  • 3. Separating a Solid from Solid. . . Filtration I t i s u s e d t o s e p a r a t e o n e s o l u b l e s o l i d a n d a n o t h e r s o l i d . Ho w d o we u s e f i l t r a t i o n t o s e p a r a t e t wo s o l i d s ? A mi x t u r e o f t w o s o l i d s c a n a l s o b e s e p a r a t e d b y f i l t r a t i o n i f o n e o f t h e m a r e s o l u b l e i n a s o l v e n t b u t t h e o t h e r i s n o t . Fo r e x a mp l e , a mi x t u r e o f s a l t a n d s a n d c a n b e s e p a r a t e d b y f i l t r a t i o n u s i n g wa t e r a s t h e
  • 4. E x p e r i me n t 3 T o s e p a r a t e a mi x t u r e o f c o mmo n t a b l e s a l t a n d s a n d Pr o c e d u r e : 1) P o u r s o m e d i s t i l l e d w a t e r i n t o t h e mi x t u r e o f c o mmo n t a b l e s a l t a n d s a n d . S t i r a n d w a r m t h e mi x t u r e . 2) P o u r t h e w a r m m i x t u r e i n t o a f i l t e r f u n n e l l i n e d wi t h f i l t e r p a p e r . Co l l e c t t h e f i l t r a t e i n a c o n i c a l f l a s k (F i g . 3.14). 3) Wa s h t h e r e s i d u e w i t h a l i t t l e d i s t i l l e d w a t e r t o r e mo v e a l l t h e s a l t s o l u t i o n f r o m i t . Th e r e s i d u e i s s a n d . 4) P o u r t h e f i l t r a t e i n t o a n e v a p o r a t i n g d i s h a n d e v a p o r a t e t h e f i l t r a t e t o d r y n e s s (F i g . 3.15). T h e w h i t e s o l i d l e f t i n t h e e v a p o r a t i n g d i s h i s s a l t .
  • 5. A n o t h e r E x a mp l e : To s e p a r a t e s a l t a n d c h a l k p o wd e r -D i s s o l v e t h e mi x t u r e u s i n g d i s t i l l e d wa t e r . -T h e s a l t w i l l d i s s o l v e i n wa t e r wh i l e t h e s a n d wi l l r e ma i n i n t h e b e a k e r . -T h e f i l t e r p a p e r o n l y a l l o ws t h e s o l u t i o n t o p a s s t h r o u g h .
  • 6. Cr y s t a l l i z a t -C o l l e c t t h e i t o an e a n d p l f i l r t a c e i t i n t o a n e v a p o r a t i n g d i s h . -E v a p o r a t e t h e wa t e r / s o l v e n t u n t i l t h e s o l u t i o n i s s a t u r a t e d . (D o n o t h e a t t o d r y n e s s ) -C o o l t h e s o l u t i o n a n d c r y s t a l s wi l l
  • 7. Separating a Solid from a Liquid. . . Decanting The simplest way to separate the water from the pebbles is to just pour the water away. This method is called decanting (Fig 3.10) We use decanting to separate a dense, insoluble solid from a liquid. Decanting is carried out everyday during many activities. For example during cooking, water is poured off various cooked foods by decanting.
  • 8. Filtration To separate sand from water, we use a method known as filtration. In general, we use filtration to separate small solid particles from liquid. Examples of small solid particles include sand, clay, dust particles and precipitates (small solid particles produced in a liquid by chemical reactions) How can we remove a precipitate from a reaction mixture by filtration? A white precipitate of lead (II) sulfate is produced when we add sodium sulfate
  • 9.
  • 10. A s o l i d c a n b e s e p a r a t e d f r o m a l i q u i d b y f i l t r a t i o n b e c a u s e t h e f i l t e r p a p e r a c t s a s a s i e v e . A l i q u i d c a n p a s s t h r o u g h t h e p o r e s (s ma l l h o l e s ) o f t h e f i l t e r p a p e r b u t a s o l i d c a n n o t d o s o . Up o n f i l t r a t i o n , t h e s o l i d t h a t r e ma i n s o n t h e f i l t e r p a p e r i s c a l l e d t h e r e s i due . Th e l i q u i d o r s o l u t i o n t h a t p a s s e s t h r o u g h t h e f i l t e r p a p e r i s c a l l e d t h e f i l t r a t e .
  • 11. Evaporation to Dryness and Crystallization When a solid is insoluble in water, the easiest way to separate it from a liquid is by filtration. However, many substances, like common salt, dissolve in water to form solutions. To separate such substances, we evaporate water from the solution. This separation technique is called evaporation to dryness. Fro example, when we evaporate salt solution to dryness, we recover solid salt. This method can be used to recover salt from seawater. However, many substances decompose when they are heated strongly. For example, sugar will decompose to give water and carbon when it is heated strongly. Most crystals, such as copper (II) sulfate crystals, give off water to become powders when heated. For such substances, evaporation to dryness is nota good method of purification. Also, when all the water is removed during evaporation, any soluble impurities present will be left on the crystals.
  • 12. The best method of obtaining a pure solid sample solution is called crystallization. How do we purify by crystallization? In crystallization, water is removed by heating the solution. Heating is stopped at the stage when a hot saturated solution is formed. If the resulting solution is allowed to cool to room temperature, the dissolved solid will be formed as pure crystals. How do we test for a saturated solution? A clean glass rod can be used to test whether a solution is saturated. It is dipped into the solution and removed. There will be a small amount of solution on the rod. If small crystals form on the rod as the solution cools, the solution is saturated. The solution is at its saturation point or crystallization point. Example: Obtaining copper (II) sulfate crystals from copper (II) sulfate solution Flowchart below shows the steps involved. Heat until the solution Copper (II) sulfate is saturated Saturated copper (II) solution sulfate solution Allow solution to cool Copper (II) sulfate Copper (II) sulfate Filter the mixture crystals + solution solution (contains soluble impurities)
  • 13. Websites for extra information : & http://www.youtube.com/watch?v=aFONmzLQJSY
  • 14. Done by: Chew Yun Jin (3) 3H/2011 1)Chemistry Matters (Marshall Cavendish) textbook 2) www.chemcompass.pbwo rks.com 3) www.google.com