LABORATORY REPORT INORGANIC

CHEMISTRY

EXPERIMENT 1

COURSE CODE

: CHM260

TITLE AND NUMBER OF EXPERIMENT

CATIONS Ag+, Fe3+, Cu2+ and Ni2+

: QUALITATIVE ANALYSIS OF

STUDENTS NAME

: KU SYAZAHANI BINTI KU RUSLAN

MATRIC NUMBER

: 2014432986

GROUP

: RAS1205C

LECTURERS NAME

: MADAM CHE FARIDAH OSMAN

DATE PERFORMED

: 15 JULY 2016

DATE SUBMIT

: 22ND AUGUST 2016

OBJECTIVES

To understand the rationale and the procedure behind the separation for
various cation.
To determine cation present in the unknown solution using established
schemes.

INTRODUCTION
HEATING SOLUTIONS
It is necessary to heat a solution to speed up the reaction. Heat the test tubes
in a boiling water bath. Set up this water bath when beginning work in the lab
because it may take time to heat the water bath to the appropriate temperature.
STIRRING SOLUTIONS
Each time a reagent is added to the test tube, the solutions needs to be
stirred. A stirring rod that is flattened to the bottom can be used as the plunger to
effectively mix solutions in a narrow test tubes.
SEPARATING SOLIDS FROM SOLUTIONS
Centrifuge the solutions so that the solid settles at the bottom of the test
tubes. Let the centrifuge spin for 30 minutes and the supernatant liquid can be
decanted from the precipitate.
1. Never fill the centrifuge tubes to its maximum capacity. Keep liquids level at
least 1cm from the top.
2. Label all centrifuge tubes before inserting to avoid mix-up.
3. Place the test tubes in a symmetrical fashion, the objective being to keep the
rotor balanced and fill all tubes to same height.
4. Follow manufacturers directions.
5. If only one test tube needs to be centrifuged, achieve balance by inserting an
additional tube containing the same volume of the liquid.
WASHING PRECIPITATES
Necessary to wash precipitates to free them from ions that might cause
confusion in later steps. Add 1mL or 2mL of water to the precipitate, stir, centrifuge
and discard the wash water.
CHECKING THE PH
To check the pH of a solution, put a piece of litmus paper or pH paper on a
clean glass plate or watch glass. Dip the stirring rod into the solution in the test tube
and touch the stirring rod the paper.
SAFETY PRECAUTIONS
Work with care and wear goggles. Wash hands thoroughly with soap and water
before leave

APPARATUS
1. Small test tube
2. Test tube racks
3. Small test tube stoppers
4. Test tube holders
5. Hot plate
6. Centrifuge
7. 250mL beakers
8. Spatula
9. Stirring rod
10. Distilled water bottle
11. Glass rod
12. Dropping pipette
13. Litmus paper
14. Vial containing unknown solution

CHEMICALS
Unknown Cationic Solutions
1. 0.05M silver nitrate AgNO3 (aq)
2. 0.05M copper (II) nitrate Cu(NO3)2 (aq)
3. 0.05M nicker nitrate Ni(NO3)2 (aq)
4. 0.05M iron (III) nitrate Fe(NO3)2 (aq)
5. 6M HCl (aq)
6. 6M HNO3 (aq)
7. 6M H2SO4 (aq)
8. 6M H2SO (aq)
9. 6M CH3COOH (aq)
10. 6M NaOH (aq)
11. 0.1M K4[Fe(CN)6]
12. 0.1M KSCN
13. Unknown solution

PROCEDURE

Experimental procedure
Qualitative Analysis of Cations
Note that the following directions are written for a known solution that contains all of
the cations. An unknown solution will probably not be able to form all the products
described in this procedure.
1. Separation of the silver from iron, copper and nickel ions.
a) 8 drops of 6M HCl was added to the solution to be analysed and
stirred. A white precipitate indicated that the Ag + ion was present.
b) The solution was centrifuged and tested with one drop of 6M HCl to
make sure the precipitate was completed. 6M HCl was continued
added if more precipitate occurred until it was completed.
c) Centrifuged, decanted (pour off), and the clear solution has been saved
into a second test tube for procedure 3.
d) The precipitate was washed by added 1mL distilled water and stirred.
The wash water was centrifuged and discarded. The precipitate was
saved for procedure 2.
2. Confirmation of silver.
a) 1mL of 6M NH3 was added to the precipitate from 1d, which is AgCl.
b) Stirred until the precipitate was completely dissolved.
c) 15 drops of 6M HCl was added to the solution. The solution was then
fumed and the reaction between the strong acid and the base gave off
heat whether or not silver was present. The test tube may get warmed.
d) The solution was stirred and tested with pH indicator paper or litmus
paper to ensure the solution was acidic. More HCl was added if it is not
acidic. White AgCl precipitate occurred in the acidic solution confirmed
the presence of silver.
e) The silver compound was disposed as directed by the instructor.
3. Separation of iron and copper from nickel.
a) 6M NaOH was added to the solution saved from procedure 1c with
stirred until the solution was basic and 3 more drops were added.
b) The test tube was stirred and placed in the hot water bath for 3
minutes. The presence of either copper or iron or both was indicated by
the formation of the precipitated.
c) The solution was then centrifuged and the clear solution was separated
from the solid. The clear solution was saved for procedure 6.
d) The precipitate was washed with a mixture of 10 drops of 6M NaOH
and 10 drops of water.
e) The wash water was centrifuged and discarded and saved for
procedure 4.
4. Separation of the iron from copper; confirmation of copper.
a) 5 drops of water were added to the precipitate from procedure 3.
b) 6 drops of 6M H2SO4 were added wised until the solution was acidic
and tested with litmus paper and stirred to dissolved the precipitate.

c) 6M aqueous NH3 was added to the solution until it was basic to litmus
and was added 1mL extra.
d) The supernatant liquid was separated from the precipitate after
centrifuged. The precipitate was kept for procedure 5. The presence of
blue Cu(NH3)42+ ion was confirmed the test for copper.
e) 6M CH3COOH, acetic acid was added to the solution contained
Cu(NH3)42+ to confirmed the test until the blue colour fades and the
solution became acidic. 2 drops of 0.1M K4[Fe(CN)6] were then added
and the presence of a red-brown precipitate of Cu[Fe(CN) 6]
reconfirmed the presence of copper.
f) The copper solution was disposed as directed by instructor.
5. Confirmation of iron.
a) The precipitate of iron hydroxide was washed from the procedure 4d.
b) 6M H2SO4 was added wised until the precipitate dissolved.
c) 5 drops of 0.1M KSCN were added to the solution. The presence of
deep red [FeSCN]2+ ion confirmed the presence of iron.
d) The iron solution was disposed as directed by the instructor.
6. Confirmation of nickel.
a) 1mL of dimethyl glyoxime solution was added to the tube and the rosered precipitate indicated the presence of nickel.

RESULT

Ag+, Fe3+, Cu2+, Ni2+

1. 6M NaOH

QUESTIONS
1. Write out the balanced net ionic equations for all the observations in the
analysis of the known cationic solution. Indicate the color of the ions and
precipitate underneath the chemical species.

Step
1.

Cation

Colour

Balanced chemical equation

2
3
4

5
6
2. What is the precipitating reagent for silver (Ag +)? Would a solution of NaCl
work as well? Why or why not?

DISCUSSION
In this experiment, the cations in samples were determined by using analysis
technique. The cations that were used are Ag+, Fe3+, Cu2+ and Ni2+. Many reagents
are used in qualitative analysis but only a few are involved in nearly every group
procedure. The four commonly used reagents are HCl, HNO 3, NaOH and NH3.

Ag+ is located in group 1. Another two are Pb 2+ and Hg2+ and cations produce
insoluble chlorides so they can be precipitated with dilute HCl, while all other cations
remain in solution. In group II, Cu2+ is here and cations produce very insoluble
sulphides so they can be precipitated by low amounts of sulphide ions. This can be
achieved by adding an acidic solution. Fe3+ and Ni2+ are in group III and cations
produce slightly soluble sulphides so they can be precipitated by relatively high
amounts of sulphide ion. This can be achieved by adding a basic solution of H 2S.
To test the silver ion, the solution was added with HCl and a precipitate of
AgCl should from if Ag+ is present. All chlorides salts are water soluble except those
of silver, mercury and lead. Then, slight excess of HCl was added to ensure the
complete precipitate. Transition elements are usually highly in coloured. A colorless
solution solution should happen if these ions are absent. To know that all the
transition metal cations are present, a colored solution will produce. An identification
of nickel is from the soluble complex ion hexaamminenickel (II) and the addition of
dimethylgloxime to this will form a red solid.

CONCLUSION
At the end of this experiment, the cation present in known solution managed to
determine by using the established schemes and the procedure behind the separation for
various cation was well understand. By knowing what a particular reaction will produce if a
specific ion is present, the ions in the solution can be identified.

REFERENCES

1. Che Faridah Osman, Cindy Tan Soo Yun. Inorganic Chemistry Laboratory
Experiments for Inorganic Experiments.
2. www.scienceinformer.com
3. https://salve.digication.com/kiley.lriviere/Data_Analysis_Conclusions