Sunteți pe pagina 1din 113

Titrations

1. No unnecessary titrations. If you have done two that are close enough,
that's already sufficient. Remember close enough means two titres within
o.10 cm^3. Example 21.50 and 21.60 is fine, 22.75 and 22.80 is fine but
23.25 and 23.40 is not enough. In such cases, perform another titration.
BURETTE: A burette has an accuracy of 0.05 cm^3. The graduations are
after every 0.10 cm^3 but you can read up to an accuracy of 0.05 cm^3. So
the maximum accepted error in the titre is 0.10 cm^3 and that's how close
the two readings we pick should be.
Graphs
1. The scale needs your values to cover at least half of the page, mind it.
2. Sharp your pencil, use 2H pencil(not HB) for graphs if available. You can
get in a good stationary shop.
3. Double check before plotting, but be real quick. One mistake in plotting
and you may mess with the whole graph.
4. Line of best fit doesn't strictly mean line only, sometimes(rarely) it could
be a curve too.
5. Always draw a triangle for gradient. The bigger the traingle, the more
accurate is your gradient.
6. Ask me now if you don't know ideas about gradient and y-intercept clearly.
7. Always write by the axis, what it represents along with its unit.
8. Independent on x-axis, dependent is y-axis. Independent is something you
are changing, depending is something you are measuring.
9. LABELLING!!!
10. Not more than 15 minutes on graph!!!
11. Even if graph is wrong, you won't lose *dherai* marks, just don't lose
hopes and work out on gradient and intercept stuffs, you will get method
markings. But never leave the questions, just fill the space even if you go
blank.
12. When they ask you to prove some relationship like T=kV or T is directly
proportional to V, write that since the graph is a straight line, the value of the
K is constant and therefore the relationship is true. DON'T FORGET IT!!!
13. If you don't have enough time, don't make all points. Make two or three

points and work out on other stuffs... Believe me, it helps if you are running
out of time.

Salt analysis (Ion test)


1. There is a trick with aluminium and lead(II) ions. Both of them give same
observation with ammonia and sodium hydroxide. To distinguish them, you
need to add HCl . If precipitate forms, it is because of lead(II) ions, otherwise
it is aluminium ions. Lead chloride is insoluble.
2. Never spend more than 45 minutes on this section.

Gas test
1. You should write the OBSERVATION of the confirmatory test whenever
needed. But to save time, you DO NOT need to perform it. Just use your
common sense of chemistry.
Example, when ZnCO3 is reacted with HCl, you know that a gas is released.
What could that be? Just think...it is CO2...Now what you need to write is
something like this(already given in the booklet) -"Colorless gas which turns
lime water milky"
Already given in the booklet, but remember NO2 is brown in color and to my
knowledge, it is very difficult to observe it. Common sense helps a lot.
Otherwise use a white paper or tile as background while observing.
2. Ammonia is pungent, very disturbing...sometimes they make you smell it.
YES, they do! Don't forget to use wet red litmus to test ammonia as well. Red
litmus turns into blue because ammonia is a base.
3. If you are not familiar with the smells of gases, you can confuse colorless
gases which smell differently. H2S, for example, smells like rotten eggs while
SO2 smells like the smoke just after you burn a match.

General Tips
1. Read carefully the names of all solutions..otherwise you will have to suffer.
Sometimes you might have to start from the beginning, it will kill your
confidence as well as time. Unlike physics practical, you need to be very

fast...It is very unlikely to happen that you will finish before time.
2. Don't spend time washing burettes and all...do it real quick!!! Like 1
burette washing in 10 seconds.
3. If you think some solutions have been mixed or there is impurity or even if
your intuition says daal mey kuch kaaala hey, then ask them to replace it!
They will not scold you like Minnu mam.
4. You make get confused with droppers. It helps making marks on
them..whatever, don't use same dropper for two solutions. Believe me, it will
affect your results.
5. If strong heating is directed, you should STRONG heat it, not just
warming...don't just write the observation fast.
6. Some examiners might be strict, they may not provide you chemicals
again until empty. Be careful in spending.
7. Use rationally pipette, burette or measuring cylinder.
8. Quote from the syllabus:
"Candidates should normally record burette readings to the nearest
0.05 cm^3 and temperature readings to the nearest 0.5 C when
using thermometer calibrated in 1 C intervals, and to the nearest 0.1
C when the interval is 0.2 C"
9. Talking about errors, an example:
Error in any instrument is half of the smallest unit you can read on it. For
instance, the stopwatch we had in the lab had the smallest unit as a 0.01s so
the error in the readings read would be +/- 0.005s.
Now you can find the uncertainty using the following formula, it might give
you an understanding why it depends on the size of the value you measure.
Ex. If I measure a value of 50s using the same stopwatch as mentioned
before with the error 0.005s. Then,
Uncertainty = [(error)/(my measured value)]*100
= [0.005/50]*100
= 0.01 percent.
But it is much more complex due to human reaction time in stopwatchs. They
won't ask you, hopefully. :)

7. Lastly, even if the practical goes horrible(like with me), don't get your
hopes down. You can easily manage to get 'a' if you work good on P1 and P2.
I've seen students with 'U' on P3, still they managed to get overall 'a'. :)

c
   
 
   
        
           
                          

             


      
                        



  
                    
 
 
         !
         "   
  
   !
 
         
     

c 
x  $!%    
     
   $!% 
 
x  $!%    
     $!% 
   $!% 
 
& '     
        (
 
   
     

 
         
     
       
     
 

 $!%    
     


 $!% $
    
  %
$&     %
     
  

 $!%
  


 
G 
$!% $
 
 
       %
 +   
  
    
  
),&c$G%),&c)$ % - c)$%
 +   
  
  
 
   '

# 
#   

    

 
#   
 
    )  

#     *
    
      )
   

 

#  


 

c
)x$&c%) )xc$ % -.&c)$% - c)$%

 
x           
             
       /  
 0     
   
&                     

   
       /  

1
1 

!  $   %

! 2  $ 2 %
0 
"   $   %

#  


&,1)G )/)-

 
  
  

r   1            
   
     
      
 
    
 


 
 
3 -    * 
 
      


3 -    ) 
 2
      



c 
/ $!% $  
    %

  
 (
 $!%
/ $!% $  
    %

  
 (
 $!%

# 
#     
    

#    

  +  '


&)1c$G% - )Gc.$+% &)Gc.$+% - )c$% - 1c)$%
11c$G% - )1$%11)$+% - )c$% - 1c)$%
               
 
3 
  
  
       

c 
/ $     %
$!%

# 
#  
    

c
 

x     
  
 



 
 $!%
   
$!%
c    $!%

  



  

#    
#  
    

r   &c              


  
    
      
   
  
              
1
 
c 
r
  &c   
   
  $!%
   '
/ 
  
  
 
r
 $!%
  
 
c    
  
    1
 +     

   1  '

# 
  

   
 



r
 



   
   




&$% - 1$% &.1$G%



 
  
  

                             
  
 


  
 
3       
       '
    
      



c   
  
 
  


3      


c 
/ $!%  
$

  % 
$!%  
$   

 %
r
 $!%
0  
  $!%
/ 
   $!%

3    

3  
G 


"  
!  
/ 
 

G 

$!% 
2   $!%

# 
     
 
#    

     

 
/ 
  
#    

    
#
G
    
#   

c

 

 
 
 



3                          
         
             



 
3      
    
     
     '   
 

    $ 


 %     




c 
r   $!%
    
$!%4  
 

 $!%
1 
  $!%
   


   


   


$!%
!    $!%
  
    



# 
#    
#    

#   

G

                      
      $!%       $!%
  +         $5   1 /  #%  '
3-$+% - 52$+% 35$ %
 


   6       6  
 

   




   

c 
 




  

 

 


! 

 


# 

 

 

 

  

!"
!

  




3       1                  
 


c
c 
# 
r   $!%
#   
G

 
                     
   $!%      u $!%
  +       
  '
/)-$+% - Gc.)2$+% /Gc.$ %

  

#            

  
 
3   7  $


 %  
&c  
    
 '
    
      
1 
c  
  


c 
/ $     %
r
 $!%

   $!%

# 
#    



  

3   *   6   
  6      x 
  6   
 
  6   
 
3  &c    
 

c 
r  $!%
G   $!%

# 
#  
 



#   



  +     x$c%)  6


  '
x)-$+% - )c2$+% x$c%)$ %
# 

#                    
 
c 
3   x    
/
   

$     %$!%
       
#   + 
  
 $!%
  +    
 
    '

# 
#   

c
x$G% - )-$+% x)-$+% - )$%
c   

3  
     
c 
#  
  #0   
#    
#   

8  *9
 
*  )
 
*  )
 
)  
 

$  

 

  
                 
c 
#       2
 
$!%
#    
 
$!%

# 
            

              
     


%
 
  u

      
        
 
3  
3     

c 
   

c    
 

# 
#      2
  
#    2 
 $   %
#       


    




 




 & 




 



 

 
'
& 




 



c





 



  


 



 

$ 

 
  




 



c

 cu 


c





 

 
 



 cu 

 
 
 
  
 

  
    '





 cu 
 






r

 


 



 

 



c  

 

[ [     
   





     

 [  [


c






 

 
c






 


 

    
!
  
  



 
 
'&
 

c 
 
 
 





 

[


  

   
 

 [ 



  

   
 
[  


 


  !
 
 


 
 





 
&
 

  
%  



 


 
%

 


 



 


  
 

 



c



  


 
 


  

r

!
 
 




 & 









(  


r

)
*cu& 








  


   
  
  
   

c







  

 +




 

 !
 

 


 
*cu
 


u
u,

&



 



 



 
%



 

 











 
 
 

 
 
 
c

$ 


$  

 


 

$  

 






&
    

 &
    

&
   

- 
 
    
" 
3
( : )8   $
     )8%

# 
1);    
  $ 3)    
      1c  
  %
1       
 
x     
 

3      $x2*%
x      +     

(   
x       '*  
(  x      

 
 6
   2*2 $x : <9%    
( : $<92)8% : *      $<92*% : ;8

!
          
    
    
  
  

 
(  
    6
       6      

 
 $=#%  
     
( :>.  c   *>   ;>  
 
 .   
$. 6*) : .?%      
     )2
  2)2
 
 
 
!         6          +       
             3 3G    
          
 
/
12  

3    +  (
2*
9992)?;

c
1:1   
*<<82*<.;
c2  
3      >;92)99
 c2   #          

6

 


 
c

 
 
  

 
.)




 


 




 
 
 
   

r

 +.) 

  
 
 

&

  




% 



/   


 

 






  



0 


0 

1 

     
2
 


 )
 
3

) (


4 

r




 
  
 % 

 
..4
 





 





You must record the masses and the weight of the solid to 2 decimal places.   
4). 

 
 4).4)






 



% 
%

  


 
 
 
 
%




    


  


  

  
 
%  



 
 
 

  &

 
%


 



  

c


-



   


 

 1 0 


  % 
  

 

0 
  % 

   




  


   
$

  
 



+.)


 -




  








 


 


  
 


 

/ 
 

#
 %! 

  




 



 





 


 

 

2
  


 






   -


 
5
 


  
 



...)% 

+...)



 













 

 

 
..+) 



 . )3.)3
().
  
 

  

 

  
 







 
..) 


 
% 
)

 
%





 












 
4

)
(





 (4+
+.+
34.
+++
0)



 .
4.
)4+
..
)
0

0)
(4+
)6+
)7+
)++

8
  
)



-

)6+")7+0 )7.)


2



  
..+) 




 )7) 

 ) 34)%
 
 
- 
r


 4 
 

..4

 


(  
 


 
 ".).


9 
% 
(  



".).".(. 

c
 

9 
% 
) 

.3. 
%
 
.  


 

%


..


9 
 

( 
2




)   










..)  
% 

) 





 )
 
 






%



) ( 


%







 
)7+


)++ .(.4 
 

 
 4
 


%



.7.


 


 
   

 


 

 


..

0 
 





 

!
 %    





 





   


 

% %
 
+.   

 
    
4 

  



&
*

 
 

04...
 8

 


 
+. 
%



+.
*

 

 
!0



!






+.) 4. 



) 8
  

  


  


-     
0 

 






   
   
 
      6
   6    6   
      
1  
 
         &)1c6)c   
   $2

 %
  

      
   )?; x  6 )c : )?; 
$
  &)1c% : *>8
5: *>9($0xx  )c% : 88  
 
 
     
  
 
 
         *9

0 
 

c
 

  



% 



+.) 

!
  
% 
  


%uc%


+)  
 
 c)



 


 

 



&
 

 






 
 
 
      


 


    



 

   

   0



 


  

 


 


 



 



! 

  










 
 



r



+.) uc 



 
 


 






 
 



 :(+)


!  

 

uc!"u"!"&!!"uc!
!"c)!!"(c:!


 


  



4
 



%




 



%+.)
 

  


) 
 
 4
 


 


4..) 



uc!uc"c
4 
()


 







 

 *

  




 

) .444):(+04...) ...7):
 *


;...7): ...4(:6
u


 


+. ...4(:6
 
  


 ...4(:.0..+. ..+63
)
 
 
 ;..+63 ..7):

c
'

 
 ()..7): .3.+)







 
 

u

  (46 6@







)


!
&

 


 









 


 
4 -
 
 
 
 




 
 
 %  0 
 0 

 2
 







%






 






  


 

 

 
 
 
 %  
0


% 
 


   


) -
 





  



 
 %
  





  



 
 

 
 
 
 %
 0 

 

 
!

* 


  


1  

 % 







1




 
 ".4<


  

%
 



   

  

 
    
3   
     x          6     
       
  6  9   
x   )  2             &c A    
6            
  
6

@   

+      
1

   

c
!
      

             +


   
    

    

   9* B       
  -29* B 3      
  @       ) 6 9* (@ 6
*99C
    
        
      
 @ #     *9B  6
  
    >< B      )  #
   *9B  6
  
    ).B         
#x"c03&
#    
                    
  
         G        @     
   #           
          @
        
#   
                 
  

 
   (  D
&    
  
     -2 9; 


$
 
#                        )     *)

    


  '
* r   

      
)   6  :
 (

    
 
  
 #         *'*    +  




 :
   
( 


    :
 6

 
+ 
   0

  4..

#    


!   +       
  $1Gc.%     $


  $##%  %
3&! G3       r30 c 10!G3 #G3#c&
"     
 
          
   
          

c
r      6                 
         

 
                          
       
3  
  
 '
0   

c   

   +
          
1      
=  C  
1

       F*99C

*  )
 
  .
 
)
 
)
 
)
   E ;9C *
      .8  );C
*
 

   +
&      
3              
        
     
     
 
  
   

   
3 

       99*
       
              

  
   ( 
  

"      



               


  $##%  
                       
* "        $##%   3 
          
6       3         
) "     


   

        


          
   6 

      


 x6              
6   
   
6        
   #       
             
3  
  
 '

c
r        
c   

   +
3     
1      
=  C  
1

      F*99C

)
 
  .
 
)
 
)
 
)
   E ;9C *     .8  );C
*
 

   +
&          
3    +         
&         


         
     


r
           D
/          
r
                D
        

#         $


 %   

  6 D G  
  
!     
      
          
"     
  
1        


 $##%   $

 : 8*?%  
  *

     *
        
 
           7

 $ ;;?%         6 


        
1      
3 x $ % (   
 6 *99C
r       *99CD
G
               
      

c    

c
c  
  


  
   
''

%


 
   
 

   



    
 


 


  


'  

 


  


   


%  
   
 


  
 


u)ucu"=>u)uc"uc




%  

 
u)ucu"=c>u)ccu"uc

 



    



 
 


u)ucuu)"=>u)cu)"uc







  %( 
 #




  





 

9

%
 
   
1
9 

9 %

 

 
  
  
 


 
  

 

Chemistry Unit 3B notes


Tests of ions:
Ion

Formula Test
Test 1
Heat the solid in a test tube with a
Bunsen burner.
It should decompose producing the
oxide and carbon dioxide. E.g.

Carbonate

CO3

2-

Hydrogencarbonate HCO3-

Sulphate (VI)

SO4

2-

Sulphite

SO32-

Chloride

Cl

Test for the gas using limewater


solution.

Observations

Limewater should
turn from colourless
to cloudy in the
presence of carbon
dioxide due to
precipitation of
calcium carbonate.

Test 2
Add dilute HCl to the solid.
Test for the gas evolved using
limewater solution.

Vigorous
effervescence.
Limewater should
turn from colourless
to cloudy in the
presence of carbon
dioxide due to
precipitation of
calcium carbonate.

Test
Add calcium chloride to a
hydrogencarbonate solution.

No precipitate forms
since calcium
hydrogencarbonate is
soluble.

Test
Add barium chloride solution acidified
with dilute HCl to the test solution.

White precipitate of
barium sulphate
forms.

Test
Warm the sulphite with dilute HCl.
The solution turns
Test for gases using acidified potassium green.
dichromate(VI) solution (or paper)
Test 1
Add concentrated sulphuric acid to the
solid chloride.

White steamy acidic


fumes are seen - HCl
fumes.

Test 2
Add dilute nitric acid to a solution of a
chloride to acidify the solution. This
White precipitate of
eliminates any carbonates or sulphites. AgCl forms.
Add silver nitrate to the solution.
Add dilute ammonia solution.
Solid dissolves.
Test 1
Add concentrated sulphuric acid to the
solid bromide.
Bromide

Br-

Test 2'
Add dilute nitric acid to a solution of a
bromide to acidify the solution. This
Cream precipitate of
eliminates any carbonates or sulphites. AgBr forms.
Add silver nitrate to the solution.
Add concentrated ammonia solution.
Solid dissolves.
Test 1
Add concentrated sulphuric acid to the
solid iodide.

Iodide

Steamy brownish
acidic fumes are
seen.

Purple acidic fumes


are seen. The mixture
turns to a brown
slurry.

Test 2
Add dilute nitric acid to a solution of a
iodide to acidify the solution. This
Yellow precipitate of
eliminates any carbonates or sulphites. AgI forms.
Add silver nitrate to the solution.

Solid is insoluble.

Add concentrated ammonia solution.

Test 1
Heat solid nitrate.

Nitrate

NO3-

If group 1 solid (not Li) then will


decompose to give the nitrite and
oxygen.
All other solid nitrates decompose to
give the metal oxide, nitrogen dioxide
and oxygen.

Oxygen gas is evolved


that will relight a
glowing splint.
Brown gas is seen
(NO2). Oxygen gas is
also evolved and will
relight a glowing
splint.

Test 2
Boil nitrate solution with
aluminium/Devardas alloy, in sodium
hydroxide solution.
Test vapour with red litmus paper.

Ammonium

NH4+

Test
Warm ammonium compound with
NaOH.
Test vapours immediately using damp
red litmus paper.

Litmus paper turns


blue in the presence
of ammonia.

NH
3
turns the litmus
paper blue.

Test
Dip nichrome wire in HCl.
Lithium

Li+

Dip wire in solid.


Heat wire in centre of flame.
Observe colour of flame.

A carmine red flame


is seen.

Test
Dip nichrome wire in HCl.
Sodium

Na+

Dip wire in solid.


Heat wire in centre of flame.

A yellow flame is
seen.

Observe colour of flame.


Test
Dip nichrome wire in HCl.
Potassium

K+

Dip wire in solid.

A lilac flame is seen.

Heat wire in centre of flame.


Observe colour of flame.

Magnesium

Mg2+

Test
Add NaOH solution to the magnesium
solid.

A white solid forms


which is insoluble in
excess NaOH(aq).
This is Mg(OH)2(s)

Test
Dip nichrome wire in HCl.
Ca2+

Calcium

Dip wire in solid.

A brick red flame is


seen.

Heat wire in centre of flame.


Observe colour of flame.
Test
Dip nichrome wire in HCl.
Sr2+

Strontium

Dip wire in solid.

A crimson red flame


is seen.

Heat wire in centre of flame.


Observe colour of flame.
Test
Dip nichrome wire in HCl.
Ba2+

Barium

Dip wire in solid.

A apple green flame


is seen.

Heat wire in centre of flame.


Observe colour of flame.

Tests of gases:
Name

Formula Test

Observations

Hydrogen

H2

Ignite gas.

Squeaky pop is heard.

Oxygen

O2

Place a glowing splint in a


sample of the gas.

The glowing splint relights.

Carbon
dioxide

CO2

A solution turns from colourless to


Bubble gas through
cloudy. A white (milky) precipitate of
limewater (saturated solution
calcium carbonate forms which is
of calcium hydroxide)
sparingly soluble.

Ammonia

NH3

Test for gas using damp red

Litmus paper turns blue.

litmus paper.

Chlorine

Cl2

Test 1
Test for gas using damp
litmus paper (red or blue)

Chlorine bleaches the litmus paper very


quickly.

Test 2
Test for gas using moist
starch-iodide paper.

The paper turns blue-black.

Test 3
The solution turns from colourless to
Pass gas through a solution of
orange.
a bromide.
Test 4
The solution turns from colourless to
Pass gas through a solution of brown (possibly with a black
an iodide.
precipitate, iodine).

Nitrogen
dioxide

Sulphur
dioxide

NO2

SO2

Not many tests for this gas.

The gas is brown.

Test 1
Bubble gas through a solution The solution turns from orange to
of potassium dichromate (VI) green.
dissolved in sulphuric acid.
Test 2
Bubble gas through a solution The solution turns from purple to
of potassium manganate (VII) colourless.
dissolved in sulphuric acid.

Volumetric analysis:
Volumetric analysis (titration) involves the reaction between two solutions. For one solution,
both the volume and the concentration are known; for the other, the volume only is known.
Apparatus used includes a burette, a pipette and a volumetric flask.

What is a standard solution?


A solution for which concentration is accurately known. The concentration may have been
found by a previous titration or by weighing the solute and making a solution of known volume.
Such a solution is a primary standard solution.

How is a 250cm3 standard solution prepared?

Make sure that the balance is clean and dry. Wipe it with a damp cloth.
Place the weighing bottle on the pan and take the balance (i.e. re-zero it)
Take the bottle off the balance and add solid to it. This ensures that no spillages fall on
the pan.
Take the balance of the weighing bottle + solid and find the balance of solid by
subtraction.
Replace on balance, and if the required amount is added, withdraw the mass.
When you have the required amount, write its value down immediately.
Wash out a 250cm3 volumetric flask three times using pure water.
Transfer the solid to a 250cm3 volumetric flask using a funnel, and wash out the
weighing bottle into the flask through the funnel using distilled water.
Add about 100cm3 of distilled water to the flask.
Stir the solution using a glass rod until all the solid visibly dissolves into a solution.
Wash all remaining apparatus including the glass rod, funnel and transfer the rest of this
to the flask.
Make up to 250cm3 with distilled water so that the bottom of the meniscus just touches
the 250cm3 mark.
Attach a stopper to the flask.
Shake the flask vigorously and/or invert the flask 5 or 6 times to create a solution with
uniform concentration.
Concentration of solution = mass of solid used/molar mass of solid x 1000/250 (units
moldm-3)

Using the pipette:

A glass bulb pipette will deliver the volume stated on it within acceptable limits only.
Using a pipette filler, draw a little of the solution to be used into the pipette and use this
to rinse the pipette.
Fill the pipette to about 2-3cm3 above the mark. Pipette fillers are difficult to adjust
accurately, so quickly remove the filler and close the pipette with your forefinger (not
thumb). Release the solution until the bottom of the meniscus is on the mark.
Immediately transfer the pipette to the conical flask in which you will do the titration,
and allow the solution to dispense under gravity.

Using the burette:

Making sure that the tap is shut, add about 10-15cm3 of the appropriate solution to the
burette and rinse it out, not forgetting to open the tap and rinse the jet.
Close the tap and fill the burette. A small funnel should be used to add the solution but
be careful not to overfill the funnel.
Remove the funnel, because titrating with a funnel in the burette can lead to serious
error if a drop of liquid in the funnel stem falls into the burette during the titration.
Bring the meniscus on to the scale by opening the tap to allow solution to pass through
the burette. There is no particular reason to bring the meniscus exactly to the zero
mark.
Make sure that the burette is full to the tip of the jet.
After a suitable indicator has been added to the solution in the conical flask, swirl the
flask under the burette with one hand whilst adjusting the burette tap with your other
hand.
Add the solution in the burette to the conical flask slowly, swirling the flask all the time.
As the endpoint is approached, the indicator will change colour more slowly. The titrant
should be added drop by drop near to the endpoint.
Repeat the titration until you have three concordant titres, i.e. volumes that are similar.
This means within 0.2cm3 or better if you have been careful. Taking the mean of three
tires that differ by 1cm3 or more is no guarantee of an accurate answer.

Common indicators:

Methyl orange - yellow in alkali, red in acid & orange in neutral solutions(usually the end
point of a titration)
Phenolphthalein - pink in alkali, colourless in acid.

Enthalpy change measurements:

Weigh a spirit lamp (containing a liquid alcohol) using a balance accurate to 3 decimal
places. Record the mass measured.
Use a measuring cylinder to put 100 cm3 of distilled water into a small beaker and
clamps this at a fixed height above the spirit lamp (about 2 cm).
Record the initial temperature of the water using a thermometer.
Light the lamp using a burning splint.
Heat the water using the spirit lamp until the temperature has gone up by about 10C.
Stir the water with the thermometer the whole time.
Put a cap on the spirit to stop the alcohol burning. The lid stops also stops further
evaporation of the liquid alcohol.
Reweigh the spirit lamp and record the mass.
Calculate the enthalpy change.

Possible sources of error:

There may be heat loss due to the apparatus used and heat may have dissipated
through the insulating material --> should use a polystyrene cup and insulation like a lid.
The specific heat capacity and density of water are used (and not of HCl).
The masses of solid added to the acid are ignored.
It is assumed that the specific heat capacity of the polystyrene cup is negligible.
Some heat is lost when the hydrogen or carbon dioxide are evolved in the reactions.

Organic Procedures:
Heating under reflux - This allows reactions to occur slowly, over a long period of time, without
any loss of volatile liquid. The solvent evaporates and is condensed and returns to the flask.

Many organic reactions are slow and require prolonged heating

To achieve this without loss of liquid, reaction mixtures are heated in a flask carrying a
vertical condenser.
This is heating under reflux; the solvent is condensed and returned to the flask, so the
mixture can be heated as long as desired.
To heat the round bottomed flask, either use a water bath, an oil bath or a heated plate
mantle. A Bunsen burner isnt really suitable.

Simple distillation:
To separate a volatile solvent from a mixture

Simple distillation is used where a volatile component has to be separated from a


mixture, the other components of the mixture being very much volatile or non-volatile.
The mixture is heated.
The fraction that boils is collected within the temperature range of the fraction.
(normally 1 or 2 degrees before the boiling temperature)
The condenser cools the fraction so it distils and is collected in the receiving flask.

Fractional distillation:
To separate mixtures of volatile liquids.

Re-crystallisation - Used to purify a solid material by removing both soluble and


insoluble impurities. The choice of solvent is important. The substance must be easily
soluble in the boiling solvent and much less soluble at room temperature. This ensures
the smallest possible loss of material, although some loss is inevitable with this
technique.

Re-crystallisation method:
1. Dissolve the solid in the minimum amount of boiling solvent. This ensures that the
solution is saturated with respect to the main solute but not with respect to the
impurities, which are present in much smaller amounts.
2. Filter the hot mixture through a preheated filter funnel. This removes insoluble
impurities. The hot funnel is necessary to prevent the solute crystallising and blocking
the funnel. Filtration under vacuum using a Buchner funnel is often preferred, because it
is fast.
3. Cool the hot filtrate, either to room temperature or, if necessary, in a bath of iced
water. Rapid cooling gives small crystals, slow cooling large ones. The large crystals are
often less pure.
4. Filter the cold mixture using a Buchner funnel.
5. Wash the crystals with a small amount of cold solvent. This removes any impurity
remaining on the surface of the crystals. A small amount of cold solvent is used so that
the crystals arent washed away / dont dissolve.
6. Suck the crystals as dry as possible on the filter.
7. Transfer the crystals to a desiccator to dry. Drying between filter paper is sometimes
recommended, but it is a very poor method.

Melting point determination:


This is used to determine the purity of the re-crystallisation solid. Place small amount of the
solid in the sealed end of a capillary tube. Place in the melting point apparatus. A sharp melting
point over a small range shows purity, when compared with the set-book value of a higher
melting point, that indicates an impure solid.

Organic tests:

Collect 10 cm of the samples.


Test the samples in the following order
Alkenes bromine water --> decolourises --> alkene
Alcohols Spatula of solid PCl5. Test fumes with damp litmus paper --> litmus red?
White fumes near ammonia? --> alcohol
Halogenoalkane Add NaOH, ethanol as solvent. Shake and warm for 3 minutes. Cool
and add nitric acid + silver nitrate. --> white = chloride; cream = bromide; yellow =
iodide. --> Confirm with ammonia
Alkane, the substance left is the alkane.

Group 1 and 2 reactions:


Sulphate solubility:
If a solution of any sulphate is added to a solution of a group 2 metal compound then a
precipitate is likely.
Group 2 ion in solution Effect of adding a sulphate solution
Mg2+

No precipitate, MgSO4 is soluble

Ca2+

White precipitate of CaSO4

Sr2+

White precipitate of SrSO4

Ba2+

White precipitate of BaSO4

Hydroxide solubility:
If sodium hydroxide is added to a solution of a group 2 compound then a precipitate is likely.
Group 2 ion in solution Effect of adding a hydroxide solution
Mg2+

Faint white precipitate of Mg(OH)2

Ca2+

Faint white precipitate of Ca(OH)2

Sr2+

Faint white precipitate of Sr(OH)2 on standing

Ba2+

No precipitate, Ba(OH)2 is soluble

Heating carbonates and nitrates:


Substance

Effect of heat

Lithium and all group 2 carbonates Carbon dioxide detected


Sodium and potassium carbonates No effect (except water of crystallisation may be given off)
Sodium and potassium nitrates

Oxygen only gas evolved

Lithium and all group 2 nitrates

Nitrogen dioxide and oxygen evolved

Action of heat on compounds:

Carbonates - Carbon dioxide is given off.


Hydrogencarbonates - Carbon dioxide and water formed.
Group 1 nitrates - Nitrite and oxygen formed.
Group 2 nitrates - Oxide, brown fumes of nitrogen dioxide and oxygen formed.

Distinguishing between hydrocarbons:

Alkane: Burn /oxidise/combust them. They will burn with a yellow flame and form CO2
and H2O (limited supply of CO).
Alkene: A yellow, sootier flame is produced (due to the extra carbon and higher ratio of
carbon:hydrogen).

Identifying some functional groups:

Alkene - Add to orange bromine water. The alkene will decolourise it.

Halogenalkane - Heat with sodium hydroxide solution. Acidify with dilute nitric acid and
then test with silver nitrate solution as with inorganic halides.

Alcohols or carboxylic acids containing C-OH - In a dry test tube (i.e. dry alcohol), add
PCl5. Misty fumes of HCl are produced, which turns blue litmus paper red.

Distinguishing between different classes of alcohol:


Primary - Add PCl5. Warm it with aqueous potassium dichromate (K2Cr2O7) and dilute H2SO4.
Misty fumes are given off and the colour changed from orange to green --> aldehyde.
Secondary - Misty fumes, changes to green --> ketone.
Tertiary - Misty fumes, no colour change.

Halogens are toxic and harmful by inhalation, although iodine is much less so than chlorine or
bromine, because it is a solid. Chlorine and bromine must always be used in a fume cupboard.
Liquid bromine causes serious burns an must be handled with gloves.
Ammonia is toxic. Concentrated ammonia solutions should be handled in the fume cupboard.
Concentrated mineral acids are corrosive. If spilt on the hands, washing with plenty of water is
usually enough, but advice must be sought. Acid in the eye requires immediate attention and
prompt professional medical attention.
Barium chloride solution and chromates and dichromates are extremely poisonous and so
should be used in the fume cupboard/should not be inhaled.
Sodium or potassium hydroxide or concentrated ammonia in the eye is extremely serious and
must always receive professional and immediate attention. Sodium hydroxide and other alkali
metal hydroxides are amongst the most damaging of all common substances to skin and other
tissue. Wear gloves, goggles and an apron when handling these solutions in high
concentrations.

General safety:

Toxic/carcinogenic use gloves, fume cupboard


Flammable Water baths, no naked fumes.
Harmful gases Use fume cupboard
Corrosive wear goggles/gloves
Spillage of concentrated acid wash with plenty of water.

EDEXCEL AS CHEMISTRY UNIT 3 NOTES


Specification
a) Recognise the results of reactions of compounds specifically mentioned in
Units 1 and 2 of the specification and the results of tests for simple ions:
carbonate, hydrogencarbonate, sulphate(VI), sulphite, chloride, bromide, iodide,
nitrate, ammonium, lithium, sodium, potassium, magnesium, calcium, strontium
and barium

Tests
Ion

Formula Test

Observations

Test 1
Heat the solid in a test tube with a Bunsen
burner.

Limewater should turn from


It should decompose producing the oxide and colourless to cloudy in the
presence of carbon dioxide due to
carbon dioxide. E.g.
precipitation of calcium carbonate.
Carbonate

CO32Test for the gas using limewater solution.


Test 2
Add dilute HCl to the solid.
Test for the gas evolved using limewater
solution.

Vigorous effervescence.
Limewater should turn from
colourless to cloudy in the
presence of carbon dioxide due to
precipitation of calcium carbonate.

Hydrogencarbonate HCO3-

Test
No precipitate forms since calcium
Add calcium chloride to a hydrogencarbonate
hydrogencarbonate is soluble.
solution.

Sulphate (VI)

SO42-

Test
Add barium chloride solution acidified with
dilute HCl to the test solution.

White precipitate of barium


sulphate forms.

Sulphite

SO

Test
Warm the sulphite with dilute HCl.
Test for gases using acidified potassium
dichromate(VI) solution (or paper)

The solution turns green.

Test 1
Add concentrated sulphuric acid to the solid
chloride.

White steamy acidic fumes are


seen - HCl fumes.

Chloride

Cl-

Bromide

Br-

23

Test 2
Add dilute nitric acid to a solution of a chloride
to acidify the solution. This eliminates any
White precipitate of AgCl forms.
carbonates or sulphites.
Add silver nitrate to the solution.
Solid dissolves.
Add dilute ammonia solution.

Test 1
Add concentrated sulphuric acid to the solid
bromide.

Steamy brownish acidic fumes are


seen.

Iodide

I-

Test 2'
Add dilute nitric acid to a solution of a
bromide to acidify the solution. This
eliminates any carbonates or sulphites.
Add silver nitrate to the solution.
Add concentrated ammonia solution.

Cream precipitate of AgBr forms.

Test 1
Add concentrated sulphuric acid to the solid
iodide.

Purple acidic fumes are seen. The


mixture turns to a brown slurry.

Solid dissolves.

Test 2
Add dilute nitric acid to a solution of a iodide
to acidify the solution. This eliminates any
Yellow precipitate of AgI forms.
carbonates or sulphites.
Add silver nitrate to the solution.

Solid is insoluble.

Add concentrated ammonia solution.


Test 1
Heat solid nitrate.
If group 1 solid (not Li) then will decompose
to give the nitrite and oxygen.
Nitrate

NO3-

Oxygen gas is evolved that will


relight a glowing splint.

All other solid nitrates decompose to give the Brown gas is seen (NO2). Oxygen
metal oxide, nitrogen dioxide and oxygen.
gas is also evolved and will relight
a glowing splint.
Test 2
Boil nitrate solution with aluminium/Devardas Litmus paper turns blue in the
alloy, in sodium hydroxide solution.
presence of ammonia.
Test vapour with red litmus paper.

Ammonium

NH4+

Test
NH
Warm ammonium compound with NaOH. 3
Test vapours immediately using damp
turns the litmus paper blue.
red litmus paper.
Test
Dip nichrome wire in HCl.

Lithium

Li+

Dip wire in solid.


Heat wire in centre of flame.
A carmine red flame is seen.
Observe colour of flame.
Test
Dip nichrome wire in HCl.

Sodium

Na+

Dip wire in solid.


Heat wire in centre of flame.
Observe colour of flame.

A yellow flame is seen.

Test
Dip nichrome wire in HCl.
Potassium

K+

Dip wire in solid.

A lilac flame is seen.

Heat wire in centre of flame.


Observe colour of flame.

Magnesium

Mg2+

Test
Add NaOH solution to the magnesium solid.

A white solid forms which is


insoluble in excess NaOH(aq). This
is Mg(OH)2(s)

Test
Dip nichrome wire in HCl.
Calcium

Ca2+

Dip wire in solid.

A brick red flame is seen.

Heat wire in centre of flame.


Observe colour of flame.

Test
Dip nichrome wire in HCl.
Strontium

Sr2+

Dip wire in solid.

A crimson red flame is seen.

Heat wire in centre of flame.


Observe colour of flame.

Test
Dip nichrome wire in HCl.
Barium

Ba2+

Dip wire in solid.


Heat wire in centre of flame.
Observe colour of flame.

A apple green flame is seen.

b) Recognise the chemical tests for simple gases, to include hydrogen, oxygen,
carbon dioxide, ammonia, chlorine, nitrogen dioxide and sulphur dioxide

Tests
Name

Formula Test

Observations

Hydrogen

H2

Ignite gas.

Squeaky pop is heard.

Oxygen

O2

Place a glowing splint in a


sample of the gas.

The glowing splint relights.

Carbon
dioxide

CO2

Bubble gas through limewater


(saturated solution of calcium
hydroxide)

A solution turns from colourless to cloudy. A white (milky)


precipitate of calcium carbonate forms which is sparingly
soluble.

Ammonia

NH3

Test for gas using damp red


litmus paper.

Litmus paper turns blue.

Test 1
Test for gas using damp litmus
Chlorine bleaches the litmus paper very quickly.
paper (red or blue)

Test 2
Test for gas using moist starch- The paper turns blue-black.
iodide paper.
Chlorine

Cl2
Test 3
Pass gas through a solution of a The solution turns from colourless to orange.
bromide.

Nitrogen
dioxide

Sulphur
dioxide

NO2

Test 4
Pass gas through a solution of
an iodide.

The solution turns from colourless to brown (possibly with


a black precipitate, iodine).

Not many tests for this gas.

The gas is brown.

Test 1
Bubble gas through a solution
of potassium dichromate (VI)
dissolved in sulphuric acid.

The solution turns from orange to green.

Test 2
Bubble gas through a solution
of potassium manganate (VII)
dissolved in sulphuric acid.

The solution turns from purple to colourless.

SO2

c) Describe the techniques used in volumetric analysis and enthalpy change


measurements

Volumetric analysis
Volumetric analysis (titration) involves the reaction between two solutions. For one solution, both
the volume and the concentration are known; for the other, the volume only is known. Apparatus
used includes a burette, a pipette and a volumetric flask.

What is a standard solution?


A solution for which concentration is accurately known. The concentration may have been found by
a previous titration or by weighing the solute and making a solution of known volume. Such a
solution is a primary standard solution.

How is a 250cm3 standard solution prepared?

Make sure that the balance is clean and dry. Wipe it with a damp cloth.

Place the weighing bottle on the pan and take the balance (i.e. re-zero it)

Take the bottle off the balance and add solid to it. This ensures that no spillages fall on the
pan.

Take the balance of the weighing bottle + solid and find the balance of solid by subtraction.

Replace on balance, and if the required amount is added, withdraw the mass.

When you have the required amount, write its value down immediately.

Wash out a 250cm3 volumetric flask three times using pure water.

Transfer the solid to a 250cm3 volumetric flask using a funnel, and wash out the weighing
bottle into the flask through the funnel using distilled water.

Add about 100cm3 of distilled water to the flask.

Stir the solution using a glass rod until all the solid visibly dissolves into a solution.

Wash all remaining apparatus including the glass rod, funnel and transfer the rest of this to
the flask.

Make up to 250cm3 with distilled water so that the bottom of the meniscus just touches
the 250cm3 mark.

Attach a stopper to the flask.

Shake the flask vigorously and/or invert the flask 5 or 6 times to create a solution with
uniform concentration.

Concentration of solution = mass of solid used/molar mass of solid x 1000/250 (units


moldm-3)

Using the pipette

A glass bulb pipette will deliver the volume stated on it within acceptable limits only.

Using a pipette filler, draw a little of the solution to be used into the pipette and use this to
rinse the pipette.

Fill the pipette to about 2-3cm3 above the mark. Pipette fillers are difficult to adjust
accurately, so quickly remove the filler and close the pipette with your forefinger (not thumb).
Release the solution until the bottom of the meniscus is on the mark.

Immediately transfer the pipette to the conical flask in which you will do the titration, and
allow the solution to dispense under gravity.

Using the burette

Making sure that the tap is shut, add about 10-15cm3 of the appropriate solution to the
burette and rinse it out, not forgetting to open the tap and rinse the jet.

Close the tap and fill the burette. A small funnel should be used to add the solution but be
careful not to overfill the funnel.

Remove the funnel, because titrating with a funnel in the burette can lead to serious error
if a drop of liquid in the funnel stem falls into the burette during the titration.

Bring the meniscus on to the scale by opening the tap to allow solution to pass through the
burette. There is no particular reason to bring the meniscus exactly to the zero mark.

Make sure that the burette is full to the tip of the jet.

After a suitable indicator has been added to the solution in the conical flask, swirl the flask
under the burette with one hand whilst adjusting the burette tap with your other hand.

Add the solution in the burette to the conical flask slowly, swirling the flask all the time.

As the endpoint is approached, the indicator will change colour more slowly. The titrant
should be added drop by drop near to the endpoint.

Repeat the titration until you have three concordant titres, i.e. volumes that are similar.
This means within 0.2cm3 or better if you have been careful. Taking the mean of three tires
that differ by 1cm3 or more is no guarantee of an accurate answer.

Common indicators

Methyl orange - yellow in alkali, red in acid & orange in neutral solutions(usually the end
point of a titration)

Phenolphthalein - pink in alkali, colourless in acid.

Enthalpy change measurements

Weigh a spirit lamp (containing a liquid alcohol) using a balance accurate to 3 decimal
places. Record the mass measured.

Use a measuring cylinder to put 100 cm3 of distilled water into a small beaker and clamps
this at a fixed height above the spirit lamp (about 2 cm).

Record the initial temperature of the water using a thermometer.

Light the lamp using a burning splint.

Heat the water using the spirit lamp until the temperature has gone up by about 10C. Stir
the water with the thermometer the whole time.

Put a cap on the spirit to stop the alcohol burning. The lid stops also stops further
evaporation of the liquid alcohol.

Reweigh the spirit lamp and record the mass.

Calculate the enthalpy change

Possible sources of error

There may be heat loss due to the apparatus used and heat may have dissipated through
the insulating material --> should use a polystyrene cup and insulation like a lid.

The specific heat capacity and density of water are used (and not of HCl).

The masses of solid added to the acid are ignored.

It is assumed that the specific heat capacity of the polystyrene cup is negligible.

Some heat is lost when the hydrogen or carbon dioxide are evolved in the reactions.

d) Describe the techniques used in simple organic preparations such as


distillation and heating under reflux

Heating under reflux - This allows reactions to occur slowly, over a long period of time, without any
loss of volatile liquid. The solvent evaporates and is condensed and returns to the flask.

Many organic reactions are slow and require prolonged heating

To achieve this without loss of liquid, reaction mixtures are heated in a flask carrying a
vertical condenser.

This is heating under reflux; the solvent is condensed and returned to the flask, so the
mixture can be heated as long as desired.

To heat the round bottomed flask, either use a water bath, an oil bath or a heated plate
mantle. A Bunsen burner isnt really suitable.

Simple distillation
To separate a volatile solvent from a mixture

Simple distillation is used where a volatile component has to be separated from a mixture,
the other components of the mixture being very much volatile or non-volatile.

The mixture is heated.

The fraction that boils is collected within the temperature range of the fraction. (normally 1
or 2 degrees before the boiling temperature)

The condenser cools the fraction so it distils and is collected in the receiving flask.

Fractional distillation
To separate mixtures of volatile liquids.

Re-crystallisation - Used to purify a solid material by removing both soluble and insoluble
impurities. The choice of solvent is important. The substance must be easily soluble in the
boiling solvent and much less soluble at room temperature. This ensures the smallest possible
loss of material, although some loss is inevitable with this technique.

Re-Crystallisation Method

Dissolve the solid in the minimum amount of boiling solvent. This ensures that the solution
is saturated with respect to the main solute but not with respect to the impurities, which
are present in much smaller amounts.

Filter the hot mixture through a preheated filter funnel. This removes insoluble impurities.
The hot funnel is necessary to prevent the solute crystallising and blocking the funnel.
Filtration under vacuum using a Buchner funnel is often preferred, because it is fast.

Cool the hot filtrate, either to room temperature or, if necessary, in a bath of iced water.
Rapid cooling gives small crystals, slow cooling large ones. The large crystals are often
less pure.

Filter the cold mixture using a Buchner funnel.

Wash the crystals with a small amount of cold solvent. This removes any impurity
remaining on the surface of the crystals. A small amount of cold solvent is used so that
the crystals arent washed away / dont dissolve.

Suck the crystals as dry as possible on the filter.

Transfer the crystals to a desiccator to dry. Drying between filter paper is sometimes
recommended, but it is a very poor method.

Melting point determination


This is used to determine the purity of the re-crystallisation solid. Place small amount of the solid
in the sealed end of a capillary tube. Place in the melting point apparatus. A sharp melting point
over a small range shows purity, when compared with the set-book value of a higher melting point,
that indicates an impure solid.

Organic tests

Collect 10 cm of the samples.

Test the samples in the following order

Alkenes bromine water --> decolourises --> alkene

Alcohols Spatula of solid PCl5. Test fumes with damp litmus paper --> litmus red? White
fumes near ammonia? --> alcohol

Halogenoalkane Add NaOH, ethanol as solvent. Shake and warm for 3 minutes. Cool and
add nitric acid + silver nitrate. --> white = chloride; cream = bromide; yellow = iodide. -->
Confirm with ammonia

Alkane, the substance left is the alkane.

e) recall and interpret details of the chemistry of the elements and compounds
listed in Units 1 and 2 of this specification
this includes the chemistry of Groups 1, 2 and 7 and the chemistry associated with the
organic compounds listed in topic 2.2

Sulphate solubility
If a solution of any sulphate is added to a solution of a group 2 metal compound then a precipitate
is likely.

Group 2 ion in solution

Effect of adding a sulphate solution

Mg2+

No precipitate, MgSO4 is soluble

Ca2+

White precipitate of CaSO4

Sr2+

White precipitate of SrSO4

Ba2+

White precipitate of BaSO4

Hydroxide solubility
If sodium hydroxide is added to a solution of a group 2 compound then a precipitate is likely.
Group 2 ion in solution

Effect of adding a hydroxide solution

Mg2+

Faint white precipitate of Mg(OH)2

Ca2+

Faint white precipitate of Ca(OH)2

Sr2+

Faint white precipitate of Sr(OH)2 on standing

Ba2+

No precipitate, Ba(OH)2 is soluble

Heating carbonates and nitrates


Substance

Effect of heat

Lithium and all group 2 carbonates

Carbon dioxide detected

Sodium and potassium carbonates

No effect (except water of crystallisation may be given off)

Sodium and potassium nitrates

Oxygen only gas evolved

Lithium and all group 2 nitrates

Nitrogen dioxide and oxygen evolved

Action of heat on compounds

Carbonates - Carbon dioxide is given off.

Hydrogencarbonates - Carbon dioxide and water formed.

Group 1 nitrates - Nitrite and oxygen formed.

Group 2 nitrates - Oxide, brown fumes of nitrogen dioxide and oxygen formed.

Distinguishing between hydrocarbons

Alkane: Burn /oxidise/combust them. They will burn with a yellow flame and form CO2 and
H2O (limited supply of CO).

Alkene: A yellow, sootier flame is produced (due to the extra carbon and higher ratio of
carbon:hydrogen).

Identifying some functional groups

Alkene - Add to orange bromine water. The alkene will decolourise it.

Halogenalkane - Heat with sodium hydroxide solution. Acidify with dilute nitric acid and
then test with silver nitrate solution as with inorganic halides.

Alcohols or carboxylic acids containing C-OH - In a dry test tube (i.e. dry alcohol), add
PCl5. Misty fumes of HCl are produced, which turns blue litmus paper red.

Distinguishing between different classes of alcohol


Primary - Add PCl5. Warm it with aqueous potassium dichromate (K2Cr2O7) and dilute H2SO4.
Misty fumes are given off and the colour changed from orange to green --> aldehyde.
Secondary - Misty fumes, changes to green --> ketone.
Tertiary - Misty fumes, no colour change.

f) interpret quantitative and qualitative results


See http://www.thestudentroom.co.uk/attachment.php?attachmentid=12846 for notes on
calculations.

g) devise and plan simple experiments based on the chemistry and techniques
summarised in a to e above Normally the last question on the paper. It will ask
you to identify certain compounds from four. E.g. titrations, how to make a
standard solution, how to titrate, identify QCO3 when heating it where Q is a
group 2 metal ion.

h) evaluate error in quantitative experiments see Appendix I for material


available to assist centres in teaching this area Percentage error = absolute
uncertainty/actual value x 100%

j) comment on safety aspects of experiments based on supplied data or recall of


the chemistry of the compounds listed in Units l and 2. Safety considerations
should relate to specific experiments not be of a general nature it will be
assumed that students wear eye protection during all practical work.

Halogens are toxic and harmful by inhalation, although iodine is much less so than chlorine or
bromine, because it is a solid. Chlorine and bromine must always be used in a fume cupboard.
Liquid bromine causes serious burns an must be handled with gloves.
Ammonia is toxic. Concentrated ammonia solutions should be handled in the fume cupboard.
Concentrated mineral acids are corrosive. If spilt on the hands, washing with plenty of water is
usually enough, but advice must be sought. Acid in the eye requires immediate attention and
prompt professional medical attention.
Barium chloride solution and chromates and dichromates are extremely poisonous and so should
be used in the fume cupboard/should not be inhaled.
Sodium or potassium hydroxide or concentrated ammonia in the eye is extremely serious and must
always receive professional and immediate attention. Sodium hydroxide and other alkali metal
hydroxides are amongst the most damaging of all common substances to skin and other tissue.
Wear gloves, goggles and an apron when handling these solutions in high concentrations.

General safety

Toxic/carcinogenic use gloves, fume cupboard

Flammable Water baths, no naked fumes.

Harmful gases Use fume cupboard

Corrosive wear goggles/gloves

Spillage of concentrated acid wash with plenty of water.

Chemistry 3B
Sulphate solubility
If a solution of any sulphate is added to a solution of a group 2 metal compound then a precipitate is
likely.
Group 2 ion in
solution

Effect of adding a sulphate


solution

Mg2+

No precipitate, MgSO4 is soluble

Ca2+

White precipitate of CaSO4

Sr2+

White precipitate of SrSO4

Ba2+

White precipitate of BaSO4

Hydroxide solubility
If sodium hydroxide is added to a solution of a group 2 compound then a precipitate is likely.
Group 2 ion in
solution

Effect of adding a hydroxide solution

Mg2+

Faint white precipitate of Mg(OH)2

Ca2+

Faint white precipitate of Ca(OH)2

Sr2+

Faint white precipitate of Sr(OH)2 on


standing

Ba2+

No precipitate, Ba(OH)2 is soluble

Heating carbonates and nitrates


Substance

Effect of heat

Lithium and all group 2


carbonates

Carbon dioxide detected

Sodium and potassium


carbonates

No effect (except water of crystallisation may be given


off)

Sodium and potassium nitrates

Oxygen only gas evolved

Lithium and all group 2 nitrates

Nitrogen dioxide and oxygen evolved

Action of heat on compounds

Carbonates - Carbon dioxide is given off.


Hydrogencarbonates - Carbon dioxide and water formed.
Group 1 nitrates - Nitrite and oxygen formed.
Group 2 nitrates - Oxide, brown fumes of nitrogen dioxide and oxygen formed.

Distinguishing between hydrocarbons

Alkane: Burn /oxidise/combust them. They will burn with a yellow flame and form CO2 and H2O
(limited supply of CO).

Alkene: A yellow, sootier flame is produced (due to the extra carbon and higher ratio of
carbon:hydrogen).

Identifying some functional groups

Alkene - Add to orange bromine water. The alkene will decolourise it.
Halogenalkane - Heat with sodium hydroxide solution. Acidify with dilute nitric acid and then test
with silver nitrate solution as with inorganic halides.
Alcohols or carboxylic acids containing C-OH - In a dry test tube (i.e. dry alcohol), add PCl5. Misty
fumes of HCl are produced, which turns blue litmus paper red.

Distinguishing between different classes of alcohol


Primary - Add PCl5. Warm it with aqueous potassium dichromate (K2Cr2O7) and dilute H2SO4. Misty
fumes are given off and the colour changed from orange to green --> aldehyde.
Secondary - Misty fumes, changes to green --> ketone.
Tertiary - Misty fumes, no colour change.

Specification
f) interpret quantitative and qualitative results.
g) devise and plan simple experiments based on the chemistry and techniques summarised in a to e above
Normally the last question on the paper. It will ask you to identify certain compounds from four. E.g.
titrations, how to make a standard solution, how to titrate, identify QCO3 when heating it where Q is a
group 2 metal ion.
h) evaluate error in quantitative experiments see Appendix I for material available to assist centres in
teaching this area Percentage error = absolute uncertainty/actual value x 100%
j) comment on safety aspects of experiments based on supplied data or recall of the chemistry of the
compounds listed in Units l and 2. Safety considerations should relate to specific experiments not be of a
general nature it will be assumed that students wear eye protection during all practical work.
Halogens are toxic and harmful by inhalation, although iodine is much less so than chlorine or bromine,
because it is a solid. Chlorine and bromine must always be used in a fume cupboard. Liquid bromine
causes serious burns an must be handled with gloves.
Ammonia is toxic. Concentrated ammonia solutions should be handled in the fume cupboard.
Concentrated mineral acids are corrosive. If spilt on the hands, washing with plenty of water is usually
enough, but advice must be sought. Acid in the eye requires immediate attention and prompt professional
medical attention.
Barium chloride solution and chromates and dichromates are extremely poisonous and so should be used
in the fume cupboard/should not be inhaled.
Sodium or potassium hydroxide or concentrated ammonia in the eye is extremely serious and must always
receive professional and immediate attention. Sodium hydroxide and other alkali metal hydroxides are
amongst the most damaging of all common substances to skin and other tissue. Wear gloves, goggles and
an apron when handling these solutions in high concentrations.

General safety

Toxic/carcinogenic use gloves, fume cupboard


Flammable Water baths, no naked fumes.
Harmful gases Use fume cupboard
Corrosive wear goggles/gloves
Spillage of concentrated acid wash with plenty of water.

tests
Ion

Formu
Test
la

Observations

Test 1
Heat the solid in a test tube with a Bunsen burner.
It should decompose producing the oxide and carbon
dioxide. E.g.
Carbonate

CO32-

Hydrogencarbona
HCO3te
Sulphate (VI)

Sulphite

Chloride

Bromide

Iodide

SO42-

2-

SO3

Cl-

Br-

I-

Limewater should turn from colourless


to cloudy in the presence of carbon
dioxide due to precipitation of calcium
carbonate.

Test for the gas using limewater solution.


Test 2
Add dilute HCl to the solid.
Test for the gas evolved using limewater solution.

Vigorous effervescence.
Limewater should turn from colourless
to cloudy in the presence of carbon
dioxide due to precipitation of calcium
carbonate.

Test
Add calcium chloride to a hydrogencarbonate solution.

No precipitate forms since calcium


hydrogencarbonate is soluble.

Test
Add barium chloride solution acidified with dilute HCl to
the test solution.

White precipitate of barium sulphate


forms.

Test
Warm the sulphite with dilute HCl.
Test for gases using acidified potassium dichromate(VI)
solution (or paper)

The solution turns green.

Test 1
Add concentrated sulphuric acid to the solid chloride.

White steamy acidic fumes are seen HCl fumes.

Test 2
Add dilute nitric acid to a solution of a chloride to acidify
the solution. This eliminates any carbonates or sulphites.
Add silver chloride to the solution.
Add dilute ammonia solution.

White precipitate of AgCl forms.

Test 1
Add concentrated sulphuric acid to the solid bromide.

Steamy brownish acidic fumes are seen.

Test 2'
Add dilute nitric acid to a solution of a bromide to acidify
the solution. This eliminates any carbonates or sulphites.
Add silver chloride to the solution.
Add concentrated ammonia solution.

Cream precipitate of AgBr forms.

Test 1
Add concentrated sulphuric acid to the solid iodide.

Purple acidic fumes are seen. The


mixture turns to a brown slurry.

Solid dissolves.

Solid dissolves.

Test 2
Add dilute nitric acid to a solution of a iodide to acidify the
solution. This eliminates any carbonates or sulphites.
Yellow precipitate of AgI forms.
Add silver chloride to the solution.

Solid is insoluble.

Add concentrated ammonia solution.


Test 1
Heat solid nitrate.

Nitrate

NO3-

If group 1 solid (not Li) then will decompose to give the


nitrite and oxygen.

Oxygen gas is evolved that will relight a


glowing splint.

All other solid nitrates decompose to give the metal oxide,


nitrogen dioxide and oxygen.

Brown gas is seen (NO2). Oxygen gas is


also evolved and will relight a glowing
splint.

Test 2
Boil nitrate solution with aluminium/Devardas alloy, in
sodium hydroxide solution.
Test vapour with red litmus paper.

Ammonium

NH4+

Litmus paper turns blue in the presence


of ammonia.

NH
Test
3
Warm ammonium compound with NaOH.
turns the litmus paper blue.
Test vapours immediately using damp red litmus paper.
Test
Dip nichrome wire in HCl.

Lithium

Li+

Dip wire in solid.


Heat wire in centre of flame.
A carmine red flame is seen.
Observe colour of flame.
Test
Dip nichrome wire in HCl.

Sodium

Na+

Dip wire in solid.


Heat wire in centre of flame.

A yellow flame is seen.

Observe colour of flame.


Test
Dip nichrome wire in HCl.
Potassium

K+

Dip wire in solid.

A lilac flame is seen.

Heat wire in centre of flame.


Observe colour of flame.
Magnesium

Mg2+

Test
Add NaOH solution to the magnesium solid.

A white solid forms which is insoluble


in excess NaOH(aq). This is
Mg(OH)2(s)

Calcium

Ca2+

Test

A brick red flame is seen.

Dip nichrome wire in HCl.


Dip wire in solid.
Heat wire in centre of flame.
Observe colour of flame.
Test
Dip nichrome wire in HCl.
Sr2+

Strontium

Dip wire in solid.

A crimson red flame is seen.

Heat wire in centre of flame.


Observe colour of flame.
Test
Dip nichrome wire in HCl.
Ba2+

Barium

Dip wire in solid.

A apple green flame is seen.

Heat wire in centre of flame.


Observe colour of flame.

Tests
Name

Formu
Test
la

Observations

Hydrogen

H2

Ignite gas.

Squeaky pop is heard.

Oxygen

O2

Place a glowing splint in a sample of the


gas.

The glowing splint relights.

Carbon
dioxide

CO2

Bubble gas through limewater (saturated


solution of calcium hydroxide)

A solution turns from colourless to cloudy. A white (milky)


precipitate of calcium carbonate forms which is sparingly
soluble.

Ammonia

NH3

Test for gas using damp red litmus paper.

Litmus paper turns blue.

Test 1
Test for gas using damp litmus paper (red or Chlorine bleaches the litmus paper very quickly.
blue)

Chlorine

Cl2

Test 2
The paper turns blue-black.
Test for gas using moist starch-iodide paper.
Test 3
Pass gas through a solution of a bromide.

The solution turns from colourless to orange.

Test 4
Pass gas through a solution of an iodide.

The solution turns from colourless to brown (possibly with a


black precipitate, iodine).

Nitrogen
dioxide

Sulphur
dioxide

NO2

SO2

Not many tests for this gas.

The gas is brown.

Test 1
Bubble gas through a solution of potassium The solution turns from orange to green.
dichromate (VI) dissolved in sulphuric acid.
Test 2
Bubble gas through a solution of potassium The solution turns from purple to colourless.
manganate (VII) dissolved in sulphuric acid.

Volumetric analysis
Volumetric analysis (titration) involves the reaction between two solutions. For one solution, both the
volume and the concentration are known; for the other, the volume only is known. Apparatus used
includes a burette, a pipette and a volumetric flask.

What is a standard solution?


A solution for which concentration is accurately known. The concentration may have been found by a
previous titration or by weighing the solute and making a solution of known volume. Such a solution is a
primary standard solution.

How is a 250cm3 standard solution prepared?

Make sure that the balance is clean and dry. Wipe it with a damp cloth.
Place the weighing bottle on the pan and tare the balance (i.e. re-zero it)
Take the bottle off the balance and add solid to it. This ensures that no spillages fall on the pan.
When you have the required amount, write its value down immediately.
Replace on balance, and if the required amount is added, withdraw the mass.
Wash out a 250cm3 volumetric flask three times using pure water.
Transfer the solid to a 250cm3 volumetric flask using a funnel, and wash out the weighing bottle
into the flask through the funnel.
Add about 100cm3 of distilled water to the flask.
Stir the solution using a glass rod.
Wash all remaining apparatus including the glass rod, funnel and transfer the rest of this to the
flask.
Make up to 250cm3 with distilled water so that the bottom of the meniscus just touches the
250cm3 mark.
Stopper the flask.
Shake the flask vigorously and/or invert the flask 5 or 6 times to dissolve the solid.
Concentration of solution = mass of solid used/molar mass of solid x 1000/250 (units moldm-3)

Using the pipette

A glass bulb pipette will deliver the volume stated on it within acceptable limits only.
Using a pipette filler, draw a little of the solution to be used into the pipette and use this to rinse
the pipette.
Fill the pipette to about 2-3cm3 above the mark. Pipette fillers are difficult to adjust accurately, so
quickly remove the filler and close the pipette with your forefinger (not thumb). Release the solution
until the bottom of the meniscus is on the mark.
Immediately transfer the pipette to the conical flask in which you will do the titration, and allow the
solution to dispense under gravity.

Using the burette

Making sure that the tap is shut, add about 10-15cm3 of the appropriate solution to the burette
and rinse it out, not forgetting to open the tap and rinse the jet.

Close the tap and fill the burette. A small funnel should be used to add the solution but be careful
not to overfill the funnel.
Remove the funnel, because titrating with a funnel in the burette can lead to serious error if a drop
of liquid in the funnel stem falls into the burette during the titration.
Bring the meniscus on to the scale by opening the tap to allow solution to pass through the
burette. There is no particular reason to bring the meniscus exactly to the zero mark.
Make sure that the burette is full to the tip of the jet.
After a suitable indicator has been added to the solution in the conical flask, swirl the flask under
the burette with one hand whilst adjusting the burette tap with your other hand.
Add the solution in the burette to the conical flask slowly, swirling the flask all the time.
As the endpoint is approached, the indicator will change colour more slowly. The titrant should be
added drop by drop near to the endpoint.
Repeat the titration until you have three concordant titres, i.e. volumes that are similar. This means
within 0.2cm3 or better if you have been careful. Taking the mean of three tires that differ by 1cm3 or
more is no guarantee of an accurate answer.

Common indicators

Methyl orange - yellow in alkali, red in acid (orange at end point)


Phenolphthalein - pink in alkali, colourless in acid.

Enthalpy change measurements

Weigh a spirit lamp (containing a liquid alcohol) using a balance accurate to 3 decimal places.
Record the mass measured.
Use a measuring cylinder to put 100 cm3 of distilled water into a small beaker and clamps this at a
fixed height above the spirit lamp (about 2 cm).
Record the initial temperature of the water using a thermometer.
Light the lamp using a burning splint.
Heat the water using the spirit lamp until the temperature has gone up by about 10C. Stir the
water with the thermometer the whole time.
Put a cap on the spirit to stop the alcohol burning. The lid stops also stops further evaporation of
the liquid alcohol.
Reweigh the spirit lamp and record the mass.
Calculate the enthalpy change

Possible sources of error

There may be heat loss due to the apparatus used and heat may have dissipated through the
insulating material --> should use a polystyrene cup and insulation like a lid.
The specific heat capacity and density of water are used (and not of HCl).
The masses of solid added to the acid are ignored.
It is assumed that the specific heat capacity of the polystyrene cup is negligible.
Some heat is lost when the hydrogen or carbon dioxide are evolved in the reactions.

Many organic reactions are slow and require prolonged heating

To achieve this without loss of liquid, reaction mixtures are heated in a flask carrying a vertical
condenser.
This is heating under reflux; the solvent is condensed and returned to the flask, so the mixture can
be heated as long as desired.

To heat the round bottomed flask, either use a water bath, an oil bath or a heated plate mantle. A
Bunsen burner isnt really suitable.

Simple distillation
To separate a volatile solvent from a mixture

Simple distillation is used where a volatile component has to be separated from a mixture, the
other components of the mixture being very much volatile or non-volatile.

The mixture is heated.

The fraction that boils is collected within the temperature range of the fraction. (normally 1 or 2
degrees before the boiling temperature)

The condenser cools the fraction so it distils and is collected in the receiving flask.

Fractional distillation
To separate mixtures of volatile liquids.

Re-crystallisation - Used to purify a solid material by removing both soluble and insoluble
impurities. The choice of solvent is important. The substance must be easily soluble in the boiling
solvent and much less soluble at room temperature. This ensures the smallest possible loss of
material, although some loss is inevitable with this technique.

Re-crystallisation method
1. Dissolve the solid in the minimum amount of boiling solvent. This ensures that the solution is
saturated with respect to the main solute but not with respect to the impurities, which are present
in much smaller amounts.

2. Filter the hot mixture through a preheated filter funnel. This removes insoluble impurities. The hot
funnel is necessary to prevent the solute crystallising and blocking the funnel. Filtration under
vacuum using a Buchner funnel is often preferred, because it is fast.

3. Cool the hot filtrate, either to room temperature or, if necessary, in a bath of iced water. Rapid
cooling gives small crystals, slow cooling large ones. The large crystals are often less pure.

4. Filter the cold mixture using a Buchner funnel.


5. Wash the crystals with a small amount of cold solvent. This removes any impurity remaining on the
surface of the crystals. A small amount of cold solvent is used so that the crystals arent washed
away / dont dissolve.

6. Suck the crystals as dry as possible on the filter.


7. Transfer the crystals to a desiccator to dry. Drying between filter paper is sometimes
recommended, but it is a very poor method.

Melting point determination


This is used to determine the purity of the re-crystallisation solid. Place small amount of the solid in the
sealed end of a capillary tube. Place in the melting point apparatus. A sharp melting point over a small
range shows purity, when compared with the set-book value of a higher melting point, that indicates an
impure solid.

Organic tests

Collect 10 cm of the samples.


Test the samples in the following order
Alkenes bromine water --> decolourises --> alkene

Alcohols Spatula of solid PCl5. Test fumes with damp litmus paper --> litmus red? White fumes
near ammonia? --> alcohol
Halogenoalkane Add NaOH, ethanol as solvent. Shake and warm for 3 minutes. Cool and add
nitric acid + silver nitrate. --> white = chloride; cream = bromide; yellow = iodide. --> Confirm with
ammonia
Alkane, the substance left is the alkane.

Techniques
Separating insoluble impurities from a soluble substance (Removing sand and impurities from salt solution)

Separating a mixture of immiscible liquids (Separating a mixture of water and hexane)


Water and hexane are immiscible forming 2 separate layers and are separated using a separating funnel
Separating a solvent from solution Simple distillation

Separating a liquid from a mixture of miscible liquids


Fractional distillation Separates mixtures of miscible liquids with different Bts, using a fractionating column increasing
efficiency of redistillation process, packed with inert material(glass beads) increasing surface area where vapour may condense.
- When mixture is boiled vapours of most volatile component(lowest Bt) rises into the vertical column where they condense to
liquids.
- As they descend they are reheated to Bt by the hotter rising vapours of the next component.
- Boiling condensing process occurs repeatedly inside the column so there is a temperature gradient.
- Vapours of the more volatile components reach the top of the column and enter the condenser for collection

Boiling under reflux Where reagents volatile


- condenses vapours and returns reagents to flask, prevents loss of
reactants/products, prolonged heating for slow reactions
- For preparation of aldehyde/carboxylic acid from alcohol
(1)Reason for heating the mixture but then taking the flame away
(1)provide Ea, exothermic/prevent reaction getting out of control

Separating mixtures of similar compounds in solution (Separating dyes present in a sample of ink)
Chromatogram
Chromatography Different components of the dye spread out at different rates
Using a square sheet of filter paper, spots of dye solutions are put along the baseline
The filter paper is coiled into a cylinder and placed in a tank containing a small volume of solvent
The lid is replaced on the tank, solvent rises up the filter paper
When the solvent nearly reaches the top of the filter paper, the filter paper is removed and position
of solvent marked.
Dyes A & B are either pure substances or a mixture of dyes not separated with the solvent used
Dye C is composed of A & B as the spots correspond
Colourless substances can be separated and seen by spraying/dipping the filter paper into a
locating agent which colours the spots produced

Separating a solid which sublimes, from a solid which doesnt sublime


Given a mixture of Ammonium chloride(sublimes) and sodium chloride(doesnt sublime)
Heat the mixture. Ammonium chloride turns directly to vapour but the sodium chloride remains unchanged
When the vapour is cooled solid ammonium chloride collects free from sodium chloride
A pure substance has a definite Mt, presence of impurities causes the substance to melt over a range of temperatures
Best method of separation of (1) Oil and water (2) Alcohol and water (3) Nitrogen from liquid air
(1) Separating funnel(2) Fractional distillation (3) Fractional distillation
Mixture
Compound
- Proportions of the different elements can be varied
- Different elements have to be present in fixed proportions
- Properties are those of the elements making it up
- Properties different from properties of elements making it up
- Elements can be separated by simple methods
- Difficult to separate into the elements which make it up
- No energy gained or lost when the mixture is made
- Energy usually given out/taken in when compound is formed
Sub-atomic particles Protons, neutrons and electrons which makes up the atom
Particle An atom, molecule, ion, electron or any identifiable particle RTP Room temperature and pressure
Electron A negatively charged particle, with negligible mass occupying the outer regions of all atoms
Immiscible Unable to mix, dissolve in each other, to form a homogenous mixture
Miscible Soluble in each other
(aq) Substance dissolved in water to form an aqueous solution
State symbols Physical state of the reactants at RT Aqueous(aq)
Solvent Substance in which other substances are dissolved
Solute Substance dissolved in another substance(solvent)to form a solution
Chemical species Collection of particles Distilled water Water that has been purified by distillation
Ion When number of protons and electrons are different
Atom The smallest part of an element that can exist on its own
Molecule 2 or more atoms bonded together
Element A pure substance which cant be split up by chemical
reaction
Compound Combination of elements in fixed proportions via
synthesis
In formation of a compound from ions the charges balance out
Physical properties: Mt, Bt, hardness
Compounds ending in ate ite contain oxygen, greater proportion of oxygen in the compound ending in ate

Sodium sulphate Na2SO4


Sodium sulphite Na2SO3
Compounds with prefix per contain extra oxygen
Sodium oxide
Na2O
Sodium peroxide Na2O2
Compounds with prefix thio contain a sulphur atom in place of an oxygen atom
Sodium sulphate Na2SO4
Sodium thiosulphate Na2S2O3
Metalloid Element which has properties between metals and nonmetals
- Ions in an ionic compound are tightly held together in a regular lattice, lattice energy is required to break it up and melt the substance
A metal high in the reactivity series has stable ores and the metal can be obtained only by electrolysis
A metal middle in the reactivity series doesnt form stable ores and can be extracted by reduction reactions (often with carbon)
A metal low in the reactivity series, if present in unstable ores can be extracted by heating
Decomposition Splitting up of a compound (Thermal decomposition - decomposition of a compound by heating)
Combustion is the reaction of a substance with oxygen, total mass of products is greater than the mass of the substance burned,
difference being the mass of oxygen combined
Sublimation of an element/compound is a transition from solid to gas with no intermediate stage
When a change of state takes place the temperature remains constant despite a continuing supply of energy. Latent heat is the energy
which is not being used to raise the temperature and supplies particles with the extra energy they require as the state changes(given out
when the reverse changes take place)
Fe(s) + CuSO4(aq) FeSO4(aq) + Cu(s)
Blue solution turns colourless and brown copper is deposited
A displacement reaction where a more reactive metal replaces a less reactive metal in a compound
Electrolysis of HCl(aq): 2HCl(aq) Cl2(g) + H2(g) Cathode: 2H+(aq) + 2e H2(g) Anode: 2Cl (aq)Cl2(g)+2e
Heat
Ammonium chloride NH4Cl(s)
NH3(g) + HCl(g)
Cool
A stopper from a bottle of (conc)NH3(aq) held near a stopper from a bottle of (conc)HCl acid gives a dense white smoke of NH4Cl
Synthetic Pathways(Series of reactions built up to convert one functional group into another)
Reactions of functional groups assumed to be the same whether molecules are simple or complicated
Synthesis of the product molecule possible because in any reaction of a functional group a product is formed capable of conversion
into other molecules

5.31 4.18 T
mass of G used (g)

1 Would the result for H be more accurate if the temperature of the solution were known to 3dp?
H =
kJ mol
Yes, temperature would then be known to a comparable precision to the other factors in the equation
Plan an experiment to investigate concentration on rate of a reaction Mg(s) + 2HCl(aq) MgCl (aq) + H (g)
2
2
Apparatus diagram/description/addition of Mg to acid in appropriate container
Weigh Mg/cut measured length and measure volume of acid, measure volume of H with time/time how long it takes for Mg to
2
dissolve repeat with different concentration(s) HCl repeat with same mass/length Mg and same volume HCl
one axis labelled concentration/volume H and other axis time/t axis changed to 1/t
2
if measured volume H at least two curves showing increasing rate with conc
2
if measured time to dissolve Mg one line showing time decreasing with conc or 1/t increasing with conc
Acid irritant so wear gloves or hydrogen explosive - no naked flame or Build up of pressure in syringe - attach plunger with string

(NH ) CO reacts with both 1moldm (dil)HNO and 1moldm (dil)KOH in the ratio 1:2
42 3
3
Devise an experiment to determine which of the two reactions is the more exothermic
Prepare solutions of known concentration of the solid

Suggestion of apparatus used e.g. lagged calorimeter or low mass polystyrene cup Use same volume of each solution
Measure maximum temperature change Improve reliability of results, repeat experiment Possible sources of error identified
Reaction with the greater temperature change is the more exothermic Since ammonia evolved use a fume cupboard
M = Group 1
M CO (s) + 2HCl(aq) 2MCl(aq)+CO (g)+H O(l)
2 3
2
2
Plan an experiment, results of which used to calculate the relative
molecular mass of the carbonate and identify M
3
At temp of experiment 1 mole of CO occupies a volume of 24dm
2
G a s s y rin g e
Relative atomic mass: Li = 7, C = 12, O = 16, Na = 23, K = 39, Rb = 85,
Cs = 133

Add M CO + acid and stopper flask/use suspended test tube in large flask
2 3
Mass of M CO and (final)vol of CO /when effervescence stops record volume of gas in syringe
2 3
2
Explain conversion volume of CO to moles by correct use of 24
2
Use of moles M CO = mass M CO M M CO to find M Hence find identity of M
2 3
2 3
r 2 3
r
Escape of gas before bung replaced/solid did not all react/CO soluble in acid Eye protection-acid hazard
2
Should not affect identification since even if M is slightly wrong it will still correspond to nearest Group 1 metal atomic mass
r
1
Plan an experiment to identify an acidic compound, molar mass for an acid estimated to be 88 2 g mol
What simple test would allow butenoic acid to be distinguished from the other two? Devise a plan based upon a quantitative
experiment that would allow the other two to be distinguished
CO O H
1
1
CH = CH CH COOH 86 g mol
CH CH CH COOH 88 g mol
1
2
2
3
2
2
HC O O H 90 g mol
3 structures proposed for this acid
Alkene detected using bromine water, only 1 would show decolourisation
Fixed mass of acid, Standard named alkali, Controlled method of addition, To an identified end point of a named suitable indicator,
Calculation of mole ratio
(1)A sample of NaCl was thought to contain an impurity of Ba(NO3)2 A student suggested a flame test
(a)(i)Suggest why a flame test on the mixture would not be a satisfactory way of detecting the presence of barium ions in the sample
(i) yellow/stronger/persistent Na flame Obscures/Ba flame NOT makes it difficult to distinguish between the two colours
(ii)Suggest a reagent that could be used to produce a ppt of a barium compound from a solution of the sample
(ii) (conc)H SO (solution) of any soluble sulphate (MgSO , (NH )2SO , Na SO )
2 4
4
4
4
2 4
(2)(a)X(has OH group)decolourised cold potassium manganate(VII) acidified with (dil)H SO acid, structure of X suggested by this?
2 4
(a)carbon double bond
(b)Complete oxidation of X with potassium dichromate(VI) solution and (dil)H2SO4 acid produces Y C H O structure for Y?
4 6
H

H
C

C H

C H

CO

CH

(1 )

(2 )

O H H
O
H
(b) H
(c)Structural formula for X?(c) H
X must be a secondary alcohol because ketone formed on oxidation carboxylic acid is not formed

(a)CH H Br + H O C H OH + H + Br
4 9
2
4 9
(b)Suggest why ethanol was used in the experiment (b)Solvent/silver nitrate solution in water and bromobutane immiscible
(c)Suggest a reason for the use of a water bath
(c)Reaction slow at RT/increases rate/flammable
(4)Describe tests you would use to distinguish between the following pairs of compounds including results
(a)NaNO and ammonium nitrate NH NO (a) Flame test, sodium salt gives yellow colour, ammonium salt gives no colour
3
4 3
(5)(a)1-bromobutane Bt102 C may be prepared by the reaction C H OH + NaBr + H SO C H Br + NaHSO + H O
4 9
2 4
4 9
4
2
(a)Describe how you would use distillation apparatus to give a sample of pure 1-bromobutane
(a)Heat mixture(slowly), collect only distillate produced at around 102 C at Bt of 1-bromobutane
(b)Suggest 2 reasons why the actual yield was much lower than the max yield
(b)side reactions, reaction incomplete, product lost in purification/transfers
(3)(a)Write an ionic equation for the hydrolysis of 1-bromobutane by water

M a ss lo s s /g

2 .0 0
(6)CaCO (s) + 2HCl(aq) CaCl (aq) + H O(l) + CO (g)
3
2
2
2
Experiment CaCO
HCl acid
3
1 .5 0
1 RT
Small pieces
3
3
50cm of 1moldm
2
Small pieces
3
3
50cm of 1moldm heated to
1 .0 0
E x p t.
80C
3 RT
One large
3
3
50cm of 1moldm
piece
0 .5 0
4 RT
Small pieces
3
3
50cm of 2moldm
(a)(i)Explain why there is a loss in mass as the reaction proceeds
(i)CO (g) evolved
5
10
15
2
T im e /m in
(ii)Explain the shape of the curve drawn for Experiment 1
Results of Experiment 1
(ii)Reaction(fast at first then)slows down/gives off less CO per
2
min when line is horizontal, the reaction has finished/after 6 or 7
minutes/when 1 g of CO lost
2
(b)Draw curves on the graph to represent the results you would expect for Experiments 2, 3 and 4. Label the curves 2, 3 and 4
(b)Experiment 2 steeper than 1 and same mass loss Experiment 3 less steep than 1 and same mass loss/reaction incomplete
Experiment 4 steeper than 1 and horizontal at twice mass loss
(7)Suggest one appropriate safety precaution that should be taken as ethanedioic acid is toxic (7)Safety pipette filler
2+
2+
(8)In an experiment to find , zinc CuSO4(aq) in a plastic cup Zn(s) + Cu (aq) Zn (aq) + Cu(s)
Suggest reasons why a series of temp readings is taken rather than simply initial and final readings
(8) Reason 1 Any fluctuations in temperature smoothed out / minimises reading error/allows line of best fit to be drawn
Reason 2 Able to allow for cooling effect/able to calculate more accurate temperature change/need to find highest temperature

Another Test List (If you find above one hard to read)
Flame test
1 Clean end of platinum/nichrome wire with(conc)HCl, burning off impurities in a roaring bunsen flame until theres no persistent flame colouration
2 Moisten the end of the clean wire with (conc)HCl and then dip into the sample to be tested
3 Hold the sample at the edge of a roaring bunsen flame
Lithium Carmine red
Calcium Brick red
Sodium Yellow
Strontium Crimson
Potassium Lilac
Barium Apple green
Gas
Test
Ammonia
NH3
Pungent smell, Moist litmus paper red blue, (conc)HCl at mouth of bottle, white smoke forms
Carbon dioxide
CO2
Pass through lime water, turning lime water milky
CaCO3(s) + H2O(l) + CO2(g)
Ca(HCO3)2(aq)
Limewater CO2 test Ca(OH)2(aq) + CO2(g) CaCO3(s) White ppt + H2O(l)
Chlorine
Cl2
Swimming pool smell, moist litmus paper blue red bleached
Hydrogen
H2
Lighted splint, burns with squeaky pop
Hydrogen chloride HCl
Moist litmus paper blue red
Nitrogen(IV)oxide
NO2
Brown gas, acrid smell, moist litmus paper blue red
Oxygen
O2
Glowing splint, relights
Water vapour
H2O
White anhydrous copper(II) sulphate white blue
CuSO4(s) + 5H2O(l)
CuSO4.5H2O(s)
Sulphur dioxide
Cation
Ammonium

SO2

NH4+
H+

Copper(II) Cu2+
Iron(II)

Fe2+

Or dry blue cobalt chloride paper blue pink


Acrid smell, moist litmus paper blue red
Or potassium dichromate(VI) solution/paper from orange green
Test
Add NaOH(aq)
Add NH4OH(aq)
Heat, ammonia evolved, moist litmus paper red blue
Moist litmus paper blue red
Add a carbonate, pass gas through lime water, CO2 evolved turning lime water milky
A little, blue ppt forms
A little, blue ppt forms
In excess, insoluble
In excess, dissolves and a dark blue solution forms
A little, green ppt forms
A little, green ppt forms

Iron(III)

Fe3+

Calcium

Ca2+

Magnesium

Mg2+

Aluminium

Al3+

Lead

Pb2+

Zinc

Zn2+

Anion
Carbonate pH>10
CO32
universal indicator
Hydrogen carbonate HCO3
pH 8-9
Chloride
Cl
Bromide

Br

Iodide

Nitrate

NO3

Sulphate

SO42

Sulphite

SO32

In excess, insoluble
In excess, insoluble
A little, brown ppt forms
A little, brown ppt forms
In excess, insoluble
In excess, insoluble
A little, milky suspension forms
A little, milky suspension forms
In excess, insoluble
In excess, insoluble
Distinguish Mg from Ca through flame test
A little, milky suspension forms
A little, milky suspension forms
In excess, insoluble
In excess, insoluble
A little, white ppt forms
A little, white ppt forms
In excess, dissolves giving colourless solution
In excess, insoluble
No ppt with (dil)H2SO4/cold(dil)HCl/(dil)KI/(dil)Na2S Sodium sulphide
A little, white ppt forms
A little, white ppt forms
In excess, dissolves giving colourless solution
In excess, insoluble
White ppt with (dil)H2SO4
White ppt with cold(dil)HCl
Yellow ppt with (dil)KI
Black ppt with (dil)Na2S Sodium sulphide
A little, white ppt forms
A little, white ppt forms
In excess, dissolves giving colourless solution
In excess, dissolves giving colourless solution
Test
Add (dil)HCl(aq)
Pass gas through lime water, CO2 evolved turning lime water milky
Or add group II ions, white ppt or heat/add boiling water, no gas evolved
Add (dil)HCl(aq)
Pass gas through lime water, CO2 evolved turning lime water milky
Or add metal ions
no ppt but heating causes white ppt to form or Heat/add boiling water, CO2 evolved
Acidify with (dil)HNO3(aq)
Add AgNO3(aq)
Add (dil)NH3 to ppt
White ppt AgCl forms Ppt dissolves leaving colourless solution
Acidify with (dil)HNO3(aq)
Add AgNO3(aq)
Add (conc)NH3 to ppt
Cream ppt AgBr forms Ppt dissolves leaving colourless solution
Acidify with (dil)HNO3(aq)
Add AgNO3(aq)
Add (conc)NH3 to ppt
Yellow ppt AgBr forms Ppt insoluble
Add NaOH(aq) Add Devardas alloy (powdered Zn, Al)
Heat & hold moist red litmus at mouth of test tube
NH3 evolved, litmus paper red blue
Add Barium nitrate Ba(NO3)2(aq)/chloride BaCl2(aq) Add HCl(aq)
White ppt
Insoluble
Add Barium nitrate Ba(NO3)2(aq)/chloride BaCl2(aq) Add HCl(aq)
White ppt
Dissolves
Or add (dil)HCl(aq) Heat
SO2 evolved turning potassium dichromate(VI) solution/paper from orange green

Practical List
1. Make a salt and calculate the percentage yield (hydrated nickel sulfate)
2. make a salt and calculate the percentage yield (ammonium iron(II) sulfate)
3. carry out and interpret results of simple test tube reactions
4. measuring some enthalpy changes
5. finding the enthalpy of combustion of an alcohol
6. finding an enthalpy change that cannot be measured directly
7. reaction of alkanes
8. reaction of alkenes
9. experiment to find the effect of electrostatic force on jets of liquid
10. solubility of simple molecules in different solvents
11. thermal decomposition of group 2 nitrates and carbonates
12. flame tests on compounds of group 1 and 2
13. simple acid-base titrations
14. oxidation of metal and non-metallic elements and ions by halogens
15. disproportion reactions with cold and hot alkali
16. iodine/thiosulfate titration and the determination of purity of potassium iodate(V)
17. reactions between halogens and halide ions/some reactions of the halides
18. factors that influence the rate of chemical reactions
19. effect of temperature, pressure and concentrations on equilibrium
20. reactions of alcohols
21. preparation of organic liquid (reflux and distillation)
22. preparation of a halogenoalkane from an alcohol
23. reactions of the halogenoalkanes.

GCE
Chemistry

User guide

Edexcel Advanced Subsidiary GCE in Chemistry (8CH01)


Edexcel Advanced GCE in Chemistry (9CH01)
Internal Assessment of Practical Skills
Issue 2
May 2008

Edexcel, a Pearson company, is the UKs largest awarding body, offering academic
and vocational qualifications and testing to more than 25,000 schools, colleges,
employers and other places of learning in the UK and in over 100 countries
worldwide. Qualifications include GCSE, AS and A Level, NVQ and our BTEC suite of
vocational qualifications from entry level to BTEC Higher National Diplomas,
recognised by employers and higher education institutions worldwide.
We deliver 9.4 million exam scripts each year, with more than 90% of exam papers
marked onscreen annually. As part of Pearson, Edexcel continues to invest in cuttingedge technology that has revolutionised the examinations and assessment system.
This includes the ability to provide detailed performance data to teachers and
students which helps to raise attainment.

This specification is Issue 2. Key changes are sidelined. We will inform centres of any
changes to this issue. The latest issue can be found on the Edexcel website:
www.edexcel.org.uk

References to third party material made in this specification are made in good faith.
Edexcel does not endorse, approve or accept responsibility for the content of
materials, which may be subject to change, or any opinions expressed therein.
(Material may include textbooks, journals, magazines and other publications and
websites.)
Authorised by Roger Beard
Prepared by Sarah Harrison
All the material in this publication is copyright
Edexcel Limited 2008

Contents

Introduction

1 The scheme of assessment

1.1 Activities

1.2 Conditions under which assessments are to be carried out

1.3 Materials allowed when carrying out assessment activities

1.4 Health and safety

2 Activity b: Qualitative observation

2.1 Recording observations

2.2 Making inferences from observations

3 Activity c: Quantitative measurement

3.1 Accuracy

3.2 Errors

3.3 Calculations

3.4 Graphs

3.5 Assumed laboratory skills

4 Activity d: Preparation

11

5 Activity c+d: Multi-stage experiment

12

Reference section

13

A Inorganic compounds and elements

13

Appearance

13

Flame tests

14

Heating

14

Recognition and identification of common gases

15

Action of dilute acids

15

Tests for oxidizing and reducing agents

16

Hydrogen peroxide solution

16

B Precipitates

17

Sodium hydroxide solution

17

Ammonia solution

18

Barium chloride solution

18

Silver nitrate solution

19

Concentrated sulfuric acid

19

C Organic compounds

20

Appearance

20

Solubility

20

Ignition

20

Chemical tests

21

D Spectroscopy

23

Mass spectrometry

23

Infrared spectroscopy

23

Nuclear magnetic resonance (nmr)

23

Introduction
This User guide has been written for students to help them in preparing for the tasks that are
part of the internal assessment of practical skills. Teachers may also find this information
helpful when preparing students for the assessment activities. The material contained in the
booklet does not extend the specification content, but aims to help students to succeed in the
assessment activities by:

explaining in more depth what is required in carrying out the activities, making
observations and measurements with appropriate precision and recording these
methodically

advising them how to interpret, explain, evaluate and communicate the results of the
activities clearly and logically using the relevant chemical knowledge, understanding and
appropriate specialist vocabulary.

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

1 The scheme of assessment

1.1

Activities

At both AS and A2 Level the skills being assessed in the activities are:
a

General practical competence (GPC)

(verification)

Qualitative observation

(14 marks)

Quantitative measurement

(14 marks)

Preparation

(12 marks)

The maximum mark available at both AS and A2 Level is 40.


Students will have their practical skills assessed by carrying out the assessment activities on a
number of occasions throughout the course. The assessment activities are set by Edexcel.
For activity a, the teacher is required to confirm that students have completed a range of
practicals over the whole year and developed their laboratory skills. Students must have
carried out at least five practicals in class. The practicals that the students complete must
cover the three areas of physical, organic and inorganic chemistry. These five practicals can
be either core practicals, or suitable alternatives.
The marks for activities b, c and d are awarded following the teachers application of the
mark schemes that accompany each assessed activity. Students need only carry out one
exercise for each of activities b, c and d. However they may carry out more than one. In this
case, only the highest mark for each activity will count towards the final mark out of 50.
At A2 there is the option of completing a multi-stage experiment at A2, which consists of
activities c and d together in a longer practical, which is worth 26 marks.
Teachers have the option of marking these activities or having them marked by Edexcel.

1.2

Conditions under which assessments are to be carried out

The practical assessment activities must be carried out under controlled conditions that
guarantee that students produce individual work. This includes those activities that involve
the processing of results. Students must not consult with each other during the activities.
Some activities can be completed in a laboratory session of approximately one hour. When an
activity has to be carried over to a following session students must not remove any materials,
including results and instruction sheets, from the laboratory. Instead, these must be collected
by the teacher and reissued at the beginning of the next session when the activity is to be
completed.

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

1.3

Materials allowed when carrying out assessment activities

Each activity has a cover sheet and a student brief giving full instructions for carrying out the
activity and the questions based on it.
During the activity students must not refer to books and notes although the data booklet is
required for some exercises. This User guide must not be used as a reference when carrying
out the internal assessment tasks.

1.4

Health and safety

Students must follow the health and safety rules which normally operate in their chemistry
laboratories, including the following:

eye protection must always be worn

laboratory coats must be worn when appropriate

plastic gloves must be worn when supplied for a particular exercise

all substances should be regarded as being potentially toxic and hazardous

HazChem labels (eg flammable) should be read and appropriate precautions (eg keep
liquid away from flame) taken

all substances spilled on the skin should be rinsed off immediately

chemicals must never be tasted

gases and vapours should never be smelt unless the question instructs the students to do
so, and then this should be done only with great care.

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

2 Activity b: Qualitative observation


Activity b will be assessed by tasks that include a number of tests to be carried out, usually on
a test tube scale. The instructions for each test will include details on quantities to be used,
whether heat is required and whether excess reagent should be added. The reagents used for
the tests will be limited to those included in the specification. Similarly, unknowns will be
limited to compounds containing the ions, elements and organic compounds with the
functional groups listed in the specification. As part of a task to identify an organic unknown,
spectroscopic data may be included for students to analyse. Other physical data such as
melting temperatures may also be given.
These qualitative observation tasks will change each year.

2.1

Recording observations

After a student has carried out each test, as instructed in the task, they must communicate
the results by giving a brief description of what has been observed. Possible changes that can
occur during tests are listed below, along with examples of what students should write in the
observation boxes.
Possible change

Example of observation

a colour change in solution

yellow solution turns orange

the formation of a precipitate

white precipitate (ppte is allowed) is formed

a precipitate dissolves in excess


reagent

precipitate dissolves in excess to form a green


solution

a gas is evolved

bubbles of gas or effervescence

tests on a gas

the gas turned damp red litmus paper blue

flame tests

yellow flame

a solid dissolves

dissolves to give a blue solution

a reaction is exothermic

the mixture becomes hot

a reaction is endothermic

the mixture feels cold

a coloured solution loses its colour

the yellow solution turns colourless

There are a number of common mistakes which students make when recording their
observations. The following should be avoided.

Referring to layers in test tubes. Almost certainly the presence of layers is due to
inadequate mixing of the reagents. The exception to this is when an organic liquid is mixed
with an aqueous solution, or with water, in which case layers may be a valid observation.

Describing colours with elaborate adjectives such as brown-black or blue-green. Marks are
awarded for simple descriptions of the colours of solutions and precipitates, such as black
or blue, even if there is a trace of a second colour.

Stating that a gas is evolved without making an observation such as bubbles or


effervescence.

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

Using clear instead of colourless for a solution. All solutions are clear even if coloured, eg
copper sulfate solution is clear but coloured blue, whereas sodium sulfate solution is
colourless.

2.2

Making inferences from observations

The purpose of asking students to make inferences from their observations is to test their
knowledge, understanding and evaluation of the chemistry which leads to the observations.
Activities include asking students to identify precipitates or gases formed in a test and which
are recorded as an observation. Also, students could be asked to identify the unknown
compound following a series of tests.
In some cases the test may be enough to enable students to suggest the identity of a
particular ion or functional group, but in others a number of possibilities may exist as a result
of a single test.
Example 1
The addition of aqueous ammonia to an inorganic compound produces a green precipitate. The
inference from this test alone should be iron(II) hydroxide, chromium(III) hydroxide or
nickel(II) hydroxide.
Example 2
In an organic analysis, a compound produces an orange precipitate with
2,4dinitrophenylhydrazine. The expected inference would be that the unknown compound is
an aldehyde, ketone or carbonyl compound. If a following test shows that the compound is an
aldehyde then the inference still stands, as this was valid on the basis of the
2,4dinitrophenylhydrazine test. If more is known about the compound, for example its
molecular formula and the fact that it cannot be oxidised, then it may be that the compound
can be identified as a result of the 2,4dinitrophenylhydrazine test.

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

3 Activity c: Quantitative measurement


Activity c will be assessed through tasks that involve using apparatus to make measurements
and to process the results, to draw conclusions and evaluate the procedure.
Quantitative activities could involve:

a volumetric analysis task

a simple thermochemistry task

a task to follow the rate of a reaction.

3.1

Accuracy

Unless an activity instructs students differently, they should assume that readings from
equipment and apparatus should be made with the following precision.
Apparatus

Precision of reading

pipette

one volume only of 25.0 cm3

burette

each volume to the nearest 0.05 cm3


mean titre to 0.05 cm3 or to the second decimal place

measuring cylinder

a 100 cm3 size to 5 cm3, a 10 cm3 size to 1 cm3

balance

readings should be made to 0.01 g or 0.001 g depending on the


precision of the balance

timers

normally read to the nearest second.

thermometers

0 to 100C thermometers should be read to the nearest 1.0C


0 to 50C thermometers to an accuracy of at least 0.5C

The following points are important.

When students record readings they should include the appropriate number of decimal
places. For example a burette reading of exactly 24.7 cm3 should be recorded in a results
table as 24.70 cm3.

When titres have to be averaged, the mean should be expressed to either the nearest
0.05 cm3 or to the second decimal place. Eg if a student records four titres as listed below
the mean should be calculated as:

26.50 + 26.25 + 26.60 + 26.65


= 26.5 cm3
4
If the student decides to ignore the second titre and to average the remaining three:
26.50 + 26.60 + 26.65
= 26.583
3
which should be recorded as 26.60 cm3 or as 26.58 (to the second decimal place).

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

Students should try to obtain at least two titres within 0.20 cm3, or better, of each other
and average these to obtain a mean titre. Students should make it clear which titres have
been used to obtain a mean.

A final result should only be given to the same number of significant figures as is suggested
in the exercise. For example a task to find a H value may involve a weighing of 1.56 g and
a temperature rise of 7.5C. A student who calculates a value of H from these figures
may obtain a value of 195.6843 on a calculator but this should be finally recorded as 200
kJ mol1, although 196 kJ mol1 may also be acceptable.

Units should always be included with a quantitative result.

A significant proportion of the marks awarded for a quantitative measurement activity will be
for accuracy. These marks will be awarded by comparing the students results with an
expected value.

3.2

Errors

Students should appreciate that any piece of equipment (burette, pipette, thermometer,
balance) used in a quantitative exercise has an uncertainty associated with its use. Even if the
equipment is used carefully, the uncertainty leads to an error in the reading and in the final
result.
Eg a balance has an uncertainty of 0.01 g when read to the second decimal place. A reading of
2.64 g recorded in an experiment has an error of:

0.01
100% = 0.38%
2.64
The following points will apply.

the uncertainty in the equipment


100%
the reading

The error in the reading =

Students should:

calculate the error involved in using a particular piece of equipment and state what effect
this has on the overall accuracy of the activity

understand that the percentage error would be affected by the magnitude of the quantity
being measured. There will be a greater error in weighing a mass of 2.64 g than in
weighing 8.64 g using the same balance.

Only a simple treatment of errors is needed and students will not be asked to combine
errors.

3.3

Calculations

Usually calculations will be structured. Students will be taken/guided through a series of steps
leading to a final answer. Since most of the marks for these steps will be for use of a correct
method, rather than for the numerical answer, it is important that students include their
workings even if these seem to be trivial. Marks cannot be awarded for an incorrect answer
without workings, but a correct method followed by an incorrect answer can often receive
credit. Units, if appropriate, should always be included with a quantitative result.
8

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

3.4

Graphs

For some activities students will need to treat their readings graphically.
The following are some useful points for students to consider when drawing graphs.

Put the dependent variable, the quantity being measured (eg temperature), on the yaxis.
And the pre-determined quantity (eg volume of solution) on the xaxis.

Choose the scales so that the results are spread out as far apart as the size of the grid
allows, but this should not be at the expense of using a sensible scale, eg using 1 cm on
the axis to represent 3 or 4 units might spread the readings better than using 1 cm to
represent 5 units, but the scale would be hard to read.

The origin (0,0) does not need to be included on either scale if it is not relevant,

For example if temperature readings between 21.0C and 39.0C are to be plotted there is
no need to begin the yaxis at 0. Rather it could be scaled from 20.0C to 40.0C.

Clearly label the axes with the quantity being plotted (eg time) and its units
(eg minutes).

Join the points plotted with a continuous straight line or smooth curve. Since the readings
are all subject to experimental error the line drawn may not necessarily pass through
every point. Points should never be joined by a series of short, straight lines.

3.5

Assumed laboratory skills

The instructions for carrying out a quantitative measurement activity will include the essential
points for the particular task. For example:

which chemicals to use

the quantities needed

the sequence of steps in the method

the readings to be taken.

The assessment activities will assume that students have developed a range of routine
practical skills in their course leading up to the exercise. Instructions may not, therefore,
include every step needed to gain accurate readings.
Examples of normal laboratory procedures which may not be referred to in the instructions
include:

burettes, pipettes and measuring cylinders should be rinsed with the solution they are to
contain

a pipette filler should always be used with a pipette

conical flasks and volumetric flasks should be rinsed out with distilled water

a burette should be read at eye level

a thermometer bulb must be held in the centre of a solution when temperature readings
are taken

care should be taken not to lose drops of a solution when thermometers or stirring rods are
removed from it

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

containers may need to be labelled if this has not already been done

care should be taken as to where apparatus is placed on the bench, eg temperature


measurements should not be taken in apparatus standing next to a Bunsen burner, in a
patch of sunlight or in a strong draught.

10

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

4 Activity d: Preparation
Activity d is assessed through tasks in which students follow a procedure to prepare and, in
some cases, purify an inorganic or organic compound. Marks are awarded for the student's
ability to follow laboratory procedures and to use apparatus competently and safely.
Preparations can include some of the following laboratory procedures:

distillation

heating under reflux

filtration, including under reduced pressure

purification by washing in a separating funnel

solvent extraction

drying

boiling and melting temperature determination

crystallization and recrystallization.

Following some preparations students will be asked to calculate the maximum mass of product
and a percentage yield.

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

11

5 Activity c+d: Multi-stage experiment


Instead of completing activities c and d separately, students could complete a multi-stage
experiment, which combines the two. This would be a longer practical which covers all of the
same aspects of c and d mentioned above. This would most likely be completed in two
laboratory sessions and students would have to hand in their notes and results at the end on
one session, and receive these back when they complete the practical in the second session.

12

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

Reference section

A Inorganic compounds and elements


1 Appearance

Coloured crystalline substances are usually hydrated salts of transition metals.


The colour of the solid substance may provide evidence for its identity.
Colour

Possible transition metal ions in salt

blue

copper(II)

pale green

iron(II)

green

copper(II), chromium(III), nickel(II)

purple

manganate(VII)

brown

iron(III)

pink

manganese(II)

yellow

chromate(VI)

orange

dichromate(VI)

The colours of transition metal ions in dilute, aqueous solution are shown in the table
below.
Colour

Possible identity

blue

copper(II)

green

iron(II), chromium(III), nickel(II)

brown / yellow

iron(III)

pale pink

manganese(II)

yellow

chromate(VI)

orange

dichromate(VI)

purple

manganate(VII)

colourless

zinc(II)

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

13

2 Flame tests

To carry out a flame test, a clean nichrome wire is used to mix a sample of a solid with
one drop of concentrated hydrochloric acid. The wire is held in progressively hotter
parts of a non-luminous Bunsen flame.
Flame colour

Inference

yellow

sodium ion

lilac

potassium ion

yellow-red*

calcium ion

red*

lithium or strontium ion

pale green

barium ion

Further tests would be needed to distinguish these ions.

3 Heating

14

Gases or vapours may be evolved on heating a solid compound.


Gas or vapour

Possible source

carbon dioxide

carbonates of metals other than group 1

oxygen

group 1 nitrates (other than Li)

oxygen and nitrogen


dioxide

nitrates (other than Na or K)

water

hydrated salts

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

4 Recognition and identification of common gases

Gas

Observations

oxygen

colourless gas which relights a glowing splint

carbon dioxide

colourless gas which gives a white precipitate with


limewater (calcium hydroxide solution)

ammonia

colourless gas which turns moist red litmus paper blue and
forms white smoke with hydrogen chloride

nitrogen dioxide

brown gas*

hydrogen

colourless gas which ignites with a pop

hydrogen chloride

steamy fumes on exposure to moist air, acidic and forms


white smoke with ammonia

chlorine

pale green gas which bleaches moist litmus paper

bromine

brown gas*

iodine

purple vapour

water vapour

turns blue cobalt chloride paper pink

Bromine dissolves in organic solvents to form a brown solution whereas nitrogen


dioxide is insoluble.

5 Action of dilute acids

When dilute sulfuric or hydrochloric acid is added to a substance a gas may be evolved
or there may be a colour change in the solution.
Action of acid

Possible source

carbon dioxide evolved

carbonate

hydrogen evolved

a metal

yellow solution turns orange

chromate(VI) to dichromate(VI)

sulfur dioxide evolved and pale yellow


precipitate formed

thiosulfate

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

15

6 Tests for oxidizing and reducing agents


Reducing agents usually:
decolourise aqueous acidified potassium manganate(VII) and
may also turn aqueous, acidified potassium dichromate(VI) from orange to green.
Reducing agents include:
iron(II) ions
iodide ions
hydrogen peroxide.
Oxidizing agents usually:
liberate iodine as a brown solution or black solid from aqueous potassium iodide.
Iodine solution gives a blue-black coloration with starch.
Oxidizing agents include:
acidified manganate(VII) ions
acidified dichromate(VI) ions
hydrogen peroxide
copper(II)ions
aqueous chlorine
aqueous bromine.

7 Hydrogen peroxide solution


Aqueous hydrogen peroxide (H2O2) can act as both an oxidizing and a reducing agent often
with the evolution of oxygen, although this may be unreliable.

16

Observation on adding H2O2

Inference

brown precipitate

manganate(VII), brown precipitate is


MnO2

purple solution is decolourised

manganate(VII) in acid solution

pale green solution turns yellow

iron(II) to iron(III) in acid solution

green precipitate turns brown

iron(II) hydroxide to iron(III) hydroxide

green alkaline solution goes yellow

chromium(III) to chromate(VI)

brown solution or black precipitate

iodine from iodide in acid solution

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

B Precipitates
When two aqueous solutions are mixed together and an insoluble compound is formed this is
known as a precipitate not a suspension. The observation that a precipitate is formed should
always be accompanied by the colour of the precipitate, even if this is white. Some reagents
should be added until they are in excess. This may result in a precipitate forming then
dissolving in excess reagent.

1 Sodium hydroxide solution

When dilute sodium hydroxide (NaOH) solution is added to a solution containing a


metal ion a precipitate of the insoluble hydroxide, eg Mn(OH)2, is usually formed.
Precipitates which are amphoteric hydroxides will dissolve in excess sodium hydroxide
to give a solution containing a complex ion, eg [Cr(OH)6]3.

Students should assume that aqueous sodium hydroxide should be added until it is in
excess even if this is not explicitly stated in the instructions.

Observation on adding dilute


NaOH

Observation on adding
excess dilute NaOH

Likely ion

green precipitate

precipitate dissolves to a
green solution

chromium(III)

off-white precipitate which


darkens on exposure to air

precipitate is insoluble

manganese(II)

green precipitate which turns


brown on exposure to air

precipitate is insoluble

iron(II)

brown precipitate

precipitate is insoluble

iron(III)

green precipitate

precipitate is insoluble

nickel(II)

blue precipitate

precipitate is insoluble

copper(II)

white precipitate

precipitate dissolves to a
colourless solution

zinc(II)

white precipitate

precipitate is insoluble

magnesium, barium,
strontium, calcium

no precipitate

sodium, potassium

no precipitate but ammonia


evolved on warming

ammonium

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

17

2 Ammonia solution

Dilute aqueous ammonia (NH3), when added to a solution containing a cation, will form
the same hydroxide precipitate as dilute sodium hydroxide solution, eg Mn(OH)2. Excess
aqueous ammonia may dissolve the precipitate to form a complex ion, eg
[Cu(NH3)4(H2O)2]2+.

Students should assume that aqueous ammonia must be added until it is in excess.

Observation on adding dilute


aqueous NH3

Observation on adding excess


dilute aqueous NH3

Likely ion

green precipitate

precipitate is soluble to give


green solution

chromium(III)

off-white precipitate

precipitate is insoluble

manganese(II)

green precipitate turning


brown

precipitate insoluble

iron(II)

brown precipitate

precipitate insoluble

iron(III)

green precipitate

precipitate dissolves to give


blue solution

nickel(II)

blue precipitate

precipitate dissolves to give


deep blue solution

copper(II)

white precipitate

precipitate dissolves to give


colourless solution

zinc(II)

white precipitate

precipitate is insoluble

magnesium

3 Barium chloride solution

Aqueous barium chloride forms precipitates of insoluble barium salts with a number of
anions but is usually used as the test for the sulfate, SO42, ion. Aqueous barium
chloride is usually used with dilute hydrochloric acid.
Anion

Precipitate

Addition of dilute HCl

colour

formula

sulfate

white

BaSO4

precipitate is insoluble

sulfite

white

BaSO3

precipitate dissolves

carbonate

white

BaCO3

precipitate dissolves with effervescence

If dilute hydrochloric acid is added to the anion solution before aqueous barium chloride
then only the sulfate will form as a precipitate.

18

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

4 Silver nitrate solution

Aqueous silver nitrate is commonly used to test for the presence of halide ions in
solution. Anions which would interfere with the test (eg carbonate) are removed by
adding dilute nitric acid before the aqueous silver nitrate.

The identity of a halide may be confirmed by the addition of aqueous ammonia, (NH3),
both dilute and concentrated.

Silver halides which dissolve in ammonia do so to form a colourless solution of the


complex ion, [Ag(NH3)2]+.
Anion

Precipitate

Addition of aqueous NH3

colour

formula

dilute

concentrated

chloride

white

AgCl

soluble

bromide

cream

AgBr

soluble in excess

soluble

iodide

yellow

AgI

insoluble

insoluble

5 Concentrated sulfuric acid

When a few drops of concentrated sulfuric acid (H2SO4) are added to a solid halide the
observed reaction products may be used to identify the particular halide ion present.
This is a potentially hazardous reaction.

It must be carried out on a small scale and in a fume cupboard.

The products in brackets will not be observed since they are colourless gases. The
halide ion may be identified without the need to test for these gases. No attempt
should ever be made to detect these gases by smell.
Halide

Observations on adding
concentrated H2SO4

Observed reaction
products

chloride

steamy fumes, vigorous reaction

HCl

bromide

steamy fumes, brown vapour,


vigorous reaction

HBr, Br2 (SO2)

iodide

steamy fumes, black solid, purple


vapour, yellow solid, vigorous
reaction

HI, I2, S, (H2S)

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

19

C Organic compounds
Students will always be told if a compound, or mixture of compounds, to be identified is
organic. Often the molecular formula, or the number of carbon atoms in a molecule, of a
compound will be given. Chemical tests may be followed by spectroscopic information.

1 Appearance
Simple organic compounds are usually colourless liquids or white solids. It is unlikely that
appearance alone will provide firm evidence for identification.

2 Solubility
Solubility of compound

Possible identity

pH of
solution

Possible
identity

dissolve in water

simple alcohols, simple


carboxylic acids,
propanone, simple
aldehydes, simple
amines and their salts

above 7

amines

below 7

carboxylic
acids,
phenols

dissolve in dilute acid


but may not dissolve in
water

amines

dissolve in aqueous
alkali but may not
dissolve in water

carboxylic acids, phenols

3 Ignition
Igniting an organic unknown on a crucible lid may help in identifying it.

20

Observation

Possible inferences

burns with a smoky flame

aromatic, unsaturated eg alkene

burns with a clean flame

saturated low molar mass compound

no residue

most lower molar mass compounds

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

4 Chemical tests
The details of how these tests are to be carried out will be included in the instructions to
students in the assessment activities.
Test

Observation

Inference

warm with acidified potassium


dichromate(VI)

orange to green
solution

primary or secondary
alcohol, aldehyde

yellow solution is
decolorised

alkene

if white
precipitate also
formed

phenol

precipitate:

halogenoalkanes:

white

CCl

cream

CBr

yellow

CI

phosphorus(V) chloride

steamy fumes of
HCl that turn damp
blue litmus paper
red

OH group in alcohols
and carboxylic acids

2,4dinitrophenylhydrazine solution

orange precipitate

C=O group in
aldehydes and
ketones

boil with Fehlings or Benedicts


solution

blue solution gives


red precipitate

aldehyde

warm with ammoniacal silver nitrate

silver mirror

aldehyde

sodium or potassium carbonate or


hydrogencarbonate solution

effervescence

carboxylic acid

add a small piece of sodium

effervescence
(bubbles), sodium
dissolves, white
solid formed

alcohol, phenol or
carboxylic acid

warm with carboxylic acid and a few


drops of concentrated sulfuric acid

ester smell, eg
glue-like

alcohol

shake with bromine water

warm with aqueous


sodium/potassium hydroxide, acidify
with dilute nitric acid then add
aqueous silver nitrate

(Tollens reagent)

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

21

Test

Observation

Inference

sodium nitrite and dilute hydrochloric


acid followed by an alkaline solution
of phenol in ice-cold conditions

orange precipitate

aromatic amine

iodine in alkaline solution

pale yellow
precipitate

methyl ketone or
ethanal,

C CH3
O
methyl secondary
alcohol or ethanol

CH CH3
OH

22

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

D Spectroscopy
Modern instrumentation plays a vital role in the characterisation and identification of
molecules and ions. The sections which follow will enable interpretation of the data likely to
be presented to students.

1 Mass spectrometry
Simplified mass spectra will be given which may be interpreted in two main ways.
1

The value of the compounds relative molar mass may be obtained from the m/e value of
M+, the molecular ion. This will have the highest value of m/e. This need not necessarily
be the base peak, which is simply the most abundant ion. Questions will be set in such a
way that students will not be confused by the presence of a line due to the (M + 1) ion.

The fragmentation pattern of the spectrum gives useful information about the structure of
the molecule. For example, a peak at m/e 29 is likely to be due to the presence of a C2H5
group in the molecule. Students are reminded that, when asked, they should give
displayed structures for fragments, which must carry a positive charge also.

2 Infrared spectroscopy
This is a very powerful non-destructive technique which provides information regarding the
nature of covalent bonds within the molecule.
Students should look at the most intense absorptions to quickly gain structural clues. Table 1
provides sufficient details to enable the principal bands to be assigned. Students should
remember that absorption frequency is affected by the chemical environment and that
absorption may take place outside the range given.
The connection between structures should be recognised. For instance, an alcohol [O-H]
stretch will be accompanied by a [C-O] stretch.
Please see the Data booklet for specific IR spectroscopy data.

3 Nuclear magnetic resonance (nmr)


Nuclear magnetic resonance spectra may be included as part of an investigation into
structure. Spectra will be high resolution with possible spinspin coupling displayed.
Please see the Data booklet for specific nmr data.

1714sb130508S:\LT\PD\Support\GCE in Chemistry Intrnl Asst of Practical Skills User guide Issue 2.doc.1-28/1

User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008

23

May 2008
For more information on Edexcel and BTEC qualifications please
visit our website: www.edexcel.org.uk
Edexcel Limited. Registered in England and Wales No. 4496750
Registered Office: One90 High Holborn, London WC1V 7BH. VAT Reg No 780 0898 07

S-ar putea să vă placă și