UNIVERSITI TEKNOLOGI MARA SABAH FACULTY OF APPLIED SCIENCE

DIPLOMA IN SCIENCE
CHM360 LABORATORY REPORT
EXPERIMENT 2 : QUALITATIVE ANALYSIS OF GROUP II CATIONS GROUP MEMBER : A.ZUL RAFIQ BIN SAPILIH - 2010202814 MOHD SHAFIQ BIN MOHD KAMARI - 2010608212 AHMAD ISMI ZULFADLI BIN ISHAK 2010852022 ALEXANDER TAGANDAP 2010269582 GROUP : AS1206A1 DATE : 7th JANUARY 2012 LECTURER : MADAM GAN GIN HOON

EXPERIMENT 2 Qualitative analysis of Group II Cations : Hg22+, Cu2+, Sn2+ and Sn4+

OBJECTIVE To identify the group II cations in solutions.

INTRODUCTION

Among the most common reactions in qualitative analysis are those involving the formation or decomposition of complex ions and precipitation reactions. These reactions may be performed directly by adding the appropriate anion, or a reagent such as H 2S or NH3 may dissociate in water to furnish the anion. Strong acid may be used to dissolve precipitates containing a basic anion. Ammonia or sodium hydroxide may be used to bring a solid into solution if the cation in the precipitate forms a stable complex with NH3 or OH-. A cation is usually present as a single principal species, which may be a complex ion, free ion, or precipitate. If the reaction goes to completion the principal species is a complex ion. The precipitate is the principal species if most of the precipitate remains undissolved. If a cation forms a stable complex, addition of a complexing agent at 1M or greater generally will convert the free ion to complex ion. The dissociation constant Kd can be used to determine the extent to which a cation is converted to a complex ion. The solubility product constant Ksp can be used to determine the fraction of cation remaining in a solution after precipitation. Kd and Ksp are both required to calculate the equilibrium constant for dissolving a precipitate in a complexing agent.

CHEMICALS Solutions of Hg2+, Cu2+, Sn2+ and Sn4+, NH3, NaOH, KI, K2CrO4, HgCl2. PROCEDURE
PART A: Reactions of Group II cations.

1. Small amount of ammonia solution in dropwise was added to test tube contained small solution of cations. When precipitation formed, the color observed. Then, excess ammonia solution was added to the test tube and the solubility was observed. 2. Small amount of NaOH solution was added in dropwise to test tube containing sample of cations. When precipitate formed, the color was observed. Then, excess amount of NaOH solutions was added and the solubility was observed. 3. Small amount of Potassium Iodide, KI solution was added to a test tube containing small amount of the cations. The color of precipitate was observed. Then, excess amount of Potassium Iodide solution was added and the solubility was observed. 4. Small amount of Potassium Chromate, K2CrO4 solution was added to a test tube containing small amount of cations. The precipitate formed was recorded. Then excess amount of Potassium Chromate solution was added, the solubility of the precipitate was observed. 5. Step 1-5 is done by using two different cations which is solutions of Hg2+ and Cu2+. The color of precipitate and solubility of precipitate was recorded. 6. For Sn2+ and Sn4+, some mercury(II) Chloride, HgCl2 solution was added to the solution and the color precipitate formed was recorded.

PART B: Identification of the cations present in unknown samples.

Test as in PART A was carried out on solution B1 and Solution B2, the cations present in each solutions was identified by the color of the precipitate and its solubility of all the cations on the PART A.

RESULTS
Cations

Hg

2+

Cu2+

NH3 NaOH When NH3 When small added, colourless amount of solution turned NaOH solution to chalky with added, white precipitate. colourless solution turned When excess to light yellow NH3 added, the precipitate with dark yellow precipitate. dissolved. When NaOH added in excess, the precipitate does not dissolved. When NH3 When small added, pale blue amount of solution turn to NaOH solution dark blue with added the blue precipitate. solution turn from pale blue When excess to gel blue NH3 added, solution turn solution with blue precipitate. from dark blue to milky blue with When NaOH the precipitate added in dissolved. excess, solution turns to gelatinous precipitate. When NH3 solution added to solution of Sn2+, there is no reaction. After excess NH3 added, there is still no reaction.

KI When small amount of KI solution added, colourless solution turns to light orange with dark orange precipitate. When excess KI added, the precipitate does not dissolved. When small amount of KI solution added, pale blue solution turns to yellow solution. When excess KI added, yellow solution turns to dirty yellow solution with white precipitate formed.

K2CrO4 When small amount of yellow K2CrO4 added, there is no reaction.

HgCl2 -

Sn2+

When NaOH

solution added solution added to solution of to solution of Sn2+, there is no Sn2+,colourless reaction. solution turn to yellow solution After excess NaOH added, When excess there is still no added, there is reaction. no reaction.

When KI

When small amount of yellow K2CrO4 added, pale blue solution turn to pale yellow. After added K2CrO4 in excess, solutions turns to dirty yellow solution with reddish brown precipitate formed When solution of K2CrO4 added to solution of Sn2+, colourless solution turn to dark yellow

When

solution of HgCl2 added to solution of Sn2+, there is no reaction.

Cations

Sn

4+

NH3 When small amount of NH3 solution added, the colour of the solution change from colourless to chalky white precipitate is formed at the bottom of the test tube. When excess of NH3 solution added, the white precipitate dissolved.

NaOH When small amount of NaOH added, the colour of the solution change from colourless to cloudy and white precipitate formed. When excess amount of NaOH added, the white precipitate dissolve.

KI When small amount of KI added, the colour of the solution change from colourless to yellow. When excess amount of KI added, no reaction occur.

B1

B2

When NH3 solution added to solution of B1, there is no reaction. After excess NH3 added, there is still no reaction. When small amount of NH3 solution added, the colour of the solution change from colourless to chalky white precipitate is formed at the bottom of the test tube. When excess of NH3 solution added, the white precipitate dissolved.

solution added to solution of B1, there is no reaction. After excess NaOH added, there is still no reaction. When small amount of NaOH added, the colour of the solution change from colourless to cloudy and white precipitate formed. When excess amount of NaOH added, the white precipitate dissolve.

When NaOH

K2CrO4 When small amount of K2CrO4, the colour of the solution change from colourless to pale yellow and yellow precipitate formed. When excess amount of K2CrO4, the colour of the solution change to dark yellow and more yellow precipitate formed. When KI When solution of solution added K2CrO4 added to to solution of solution of B1, B1, colourless colourless solution turn to solution turn to yellow solution. dark yellow. When excess added, there is no reaction. When small When small amount of amount of KI K2CrO4, the added, the colour of the colour of the solution change solution from colourless change from to pale yellow colourless to and yellow yellow. precipitate When excess formed. amount of KI When excess added, no amount of reaction occur. K2CrO4, the colour of the solution change to dark yellow and more yellow precipitate formed.

HgCl2 When solution of HgCl2 added to solution of Sn4+, there is no reaction.

No reaction
occur.

No reaction
occur.

DISCUSSION

Based on the experiment carried in, for the addition of some NH3 solution to the solution of cations cause the solutions of Hg2+ and Sn4+ to turn from colourless solution to chalky solution and consist of white precipitate that is deposited on the bottom of the test tube. Next, all the test tube contained the white precipitate were added with excess amount of NH3 solutions. The results turn out that when the test tube with white precipitate that originally contain Hg2+ and Sn4+ ion, the precipitate were dissolve little by little until all of it eventually dissolved upon the addition of NH3 solution. This indicates the complex formation. For Cu2+ cation, when NH3 added, pale blue solution turns to dark blue with blue precipitate. When excess NH3 added, solution turned from dark blue to milky blue with the precipitate dissolved. While for Sn2+ cation, it shows no reaction upon the addition of NH3 solution. After excess NH3 added to Sn2+, it still shows no reaction. Therefore, based on the results we can differentiate them by different result whn NH3 added which only Hg2+ and Sn4+ cation turned to chalky with white precipitate, Cu2+ turned to dark blue with blue precipitate and Sn2+ shows no reaction. For the second test, upon the addition of small amount of NaOH solutions to Hg2+ solution cause the colourless solution turned to light yellow with dark yellow precipitate. Gel blue solution with blue precipitate was formed with addition of NaOH solution with Cu2+ solution while for addition of NaOH solution to Sn4+ solution cause the solution turn to chalky solution and white precipitate formed. For Sn2+ solution, there is no reaction upon addition of NaOH solution. After the precipitate formed, NaOH solution then added in excess to all four test tubes containing solutions of Hg2+, Cu2+, Sn2+ and Sn4+. For Sn4+ solutions, the white precipitate was dissolved and forming colourless homogeneous solution after the addition of NaOH solution that indicates the complex formation. While for both of the solutions of Hg2+ and Cu2+ the addition of NaOH solutions in excess cause the precipitate to remain and does not dissolve. For Sn2+, it still show no reaction upon addition of excess NaOH solution. Thus, for the second test, firstly the solutions of Hg2+, Cu2+, Sn2+ and Sn4+ can be compare by using small amount of NaOH solutions where dark yellow precipitate formed with Hg2+,blue precipitate for Cu2+ solution and white precipitate formed for Sn4+ solution while no reaction for Sn2+. Secondly, with addition of excess NaOH solution, homogeneous colourless solution will be formed with Sn4+ solution while precipitate remained for both solutions of Hg2+, and Cu2+ solutions.

For the third test, when small amount of KI added to the Hg2+,the colour of solution will change from colurless to light yellow and dark orange precipitate formed. When added to Cu2+ and B2, the colour of solution change from pale blue to yellow. When added to Sn2+, Sn4+ and B1, the reaction are the same which the solution change from colorless to yellow. For in excess, only Cu2+ give reaction because yellow solution turns to dirty yellow solution with white precipitate formed. For the Hg2+, the white precipitate was not dissolve and for cations Sn2+, Sn4+, B1 and B2 solution, there is no reaction that occur on this four test tube. For the fourth test, when small amount of K2CrO4, there is no reaction that occur on the test tube containing Hg2+, while in the test tube containing Sn2+ the solution change from colourless to dark yellow. In the test tube that containing Cu2+ and B1 solution, the reaction are the same which the colour of the solution change from pale blue to dark yellow. For test tube containing Sn4+ and B2 solution, the reaction also same where both of this cations and solution, the colour of the solution change from colourless to pale yellow and yellow precipitate formed. When excess of K2CrO4 added to Hg2+, still no reaction occur while in the test tube containing Cu2+, solutions turns to dirty yellow solution with reddish brown precipitate formed. For cations Sn4+ and B2 solution, both of it have same reaction which are , the colour of the solution change to dark yellow and more yellow precipitate formed. For our fifth reagent which is HgCl2, it was only added to two cations which is Sn2+ and Sn4+, but it shows no reaction upon the addition of HgCl2 to the solutions. In this experiment, we are required to identify an unknown samples which is B1 and B2 by carry out the tests using same reagent which is NH3, NaOH, KI, K2CrO4, HgCl2. According to the results, we identified B1 solution as Sn2+ while B2 solution is Sn4+. A few precautions were done to ensure our results contain less or no error. Firstly, before conducting the experiment all the test tubes were cleaned first to prevent contamination. Then, they were rinsed with little amount of the cation solutions to be used on each test tubes. Then, the tip of the dropper used for each of the solution were ensure not to touch the surface of the test tube and does not leave lie on the table after each use. It was pun inside the container of the solutions. This precaution taken to prevent contamination to the solutions.

QUESTIONS Write the equation of the following reactions:

1. Reaction between tin(IV) ion and Sodium Hydroxide (limited and excess).

Sn4+

(aq)

+ 4OH-(aq)

Sn(OH)4(s)

(limited)

Sn(OH)4(s) + 2OH-(aq)

[Sn(OH)6]2-(aq) (excess)

2. Reaction between Mercury(II) Ion and Potassium Iodide(limited and excess)

Hg2+(aq) + 3I-(aq) HgI3(aq) + I(aq)

HgI3(s) HgI

(limited) (excess)

3. Reaction between Copper(II) Ion and Potassium Iodide.

Cu2+(aq) + I-(aq)

CuI2(aq)

CONCLUSION The reagents used to identify cations give different results such as precipitate, colour and complex formation and thus can be used to identify an unknown solution. B1 solution identified as Sn2+ solution and B2 is Sn4+ solution.

REFERENCES 1. Raymond Chang and Brandon Cruickshank 2005. Chemistry Eighth Edition. McGraw-Hill International Edition. 2. Martin S.Silberberg 2009. Chemistry : The Molecular Nature of Matter and Change Fifth Edition. McGraw-Hill International Edition.