INORGANIC CHEMISTRY (CHM 3301)

NAME MATRIC NO PROGRAMME : Nur Azhani bt Ab Aziz : 156306 : Bac Sc( Hons)- Industrial Chemistry

PARTNER NAME MATRIC NO PROGRAMME

: Izwaharyanie bt Ibrahim : 156342 : Bac Sc( Hons)- Industrial Chemistry

TITLE

: Preparation Of Double Salt and Complex Salt

NO.OF EXPERIMENT : 4

DATE

: 19 September 2011

DEMONSTRATOR

EXPERIMENT 4 TITLE : PREPARATION OF DOUBLE SALT AND COMPLEX SALT OBJECTIVES : After carrying out the experiment, we are able to : 1. Synthesise double salt and complex salt using wet chemistry method. 2. Characterise and compare the physical and chemical properties between the prepared salts. INTRODUCTION : A double salt is a salt that crystallizes as a single substances but ionizes as two distinct salts when dissolved, as a carnallite KMgCl3 .6H2O. Double salts contain more than one cation or anion. They form when more than one salt is dissolved in a liquid and when together they crystallize in a regular pattern. They have their own crystal forms, which need not be the same as that of either component. Double salt has two different cations in their crystal lattice in a definite proportion and they commonly form large crystal more readily than the single salt that made them up. A well-known double salt is alum containing two cations (sodium and aluminium) and a sulfate anion. Alums are double sulphates of a monovalent cation and a trivalent cation containing 24 water of crystallization. Other example are potassium sodium tartrate and bromlite. Epsom sals are also an example of a double salt. Complex salt is formed when an addition compound is dissolve in water or organic solvent and it does not dissociate, does not give its constituent ions, and does not lose its identity with such addition compound. A complex salt is the salt of one or more complex ions, the complex part can be either cation or anion. Sometimes it also can be both anion and cation. For example, Ca3[Co(Cl)6]2 the complex part behaves as an anion and [Co(NH3)6]Cl3 the complex part behaves as a cation. In order to prepare a complex salt, a light blue precipitate of cupric hydroxide is first formed when ammonia is added to a solution of a cupric salt. Then it form a deep purplish blue solution when dissolve in excess ammonia. The color is due to the complex ion Cu (NH3)4 and the sulphate of this ion is easily obtained in solid form as the hydrated Cu (NH3)4 SO4. H2O.

METHODOLOGY : (A) Preparation of double salt , CuSO4 (NH4)2 SO4 .6H2O 7.49 g of 0.03 mol of CuSO4.5H2O + 3.96 g of 0.03 mol (NH4)2 SO4 15 ml hot water The solution was left aside to let it cool slowly

mix and dissolve

The crystal was filtered by using Buchner funnel

It was let to dried on filter paper

The crystal was weight and recorded

(B) Preparation of complex salt, Cu (NH3) SO4. H2O 6.25g CuSO4.5H2O + 6ml water + 10ml concentrated ammonia

Then, 10 ml of ethyl alcohol was added slowly

The solution was allowed to stand for an hour

It was cooled inside the ice bath

The crystal was filtered by using Buchner funnel

The crystal was wash with equal amount volume of alcohol and concentrated ammonia, followed by alcohol then ether.

The crystal was let to dried

The crystal was weight and recorded

RESULTS : For double salt, CuSO4 (NH4). 6H2O and complex salt Cu(NH3)4 SO4. H2O Double salt Weight of filter paper Weight of yield + filter paper Weight of yield Comparison between properties of double salt and complex salt Properties Colour Solubility in alcohol Solubility in water Physical state IR Type of bond N-H S-O Cu-S Cu-N UV There is a peak occur at 807.39 nm with 0.502 absorption for double salt. However for complex salt, there was no peak that can be determined. Frequency (cm-1) Double salt 3124.64 1401.40 1630.82 1099.56 Frequency (cm-1) Complex salt 3231.30 1402.32 1617.62 1112.56 Double salt Light blue Not soluble Not soluble Solid Complex salt Dark blue Soluble Slightly soluble Solid Complex salt

CALCULATION : ( A ) Preparation of double salt, CuSO4(NH4)3 SO4. 6H2O Mass determination of double salt

No. of mole of CuSO4. 5H2O = 0.03 mole Relative molecular mass CuSO4. 5H2O = 63.44 + 32.064 + 4(16.00) + 5[ 2(1.008) 16.00 ] = 249.58 g mol :: Mass of CuSO4. 5H2O used in the experiment = 0.03 x 249.58 = 7.4874 g

No. of mole of (NH4)2 SO4 = 0.03 mole Relative molecular mass of (NH4)2 SO4 = 2 [ 14.0067 + 4(1.008) ] + 32.064 + 4(16.00) = 132.14 gmol :: Mass of (NH4)2 SO4 used in experiment = 0.03 x 132.14 =3.9642 g

The equation of reaction : CuSO4. 5H2O (aq) + (NH4)2 SO4 (aq) + H2O From the equation above : CuSO4 (NH4)2 SO4. 6H2O (s)

1mole of CuSO4.5H2O 1mole of CuSO4. (NH4)2 SO4. 6H2O :: 0.03mole of CuSO4. 5H2O 0.03mole of CuSO4(NH4)2 SO4. 6H2O

Formula mass of CuSO4 (NH4)2.6H2O = 63.54 32.064+4(16.0)+2[14.0067+3(1.008)]+32.064+4(16.0)+6[2(1.008) + 16.0] = 397.8165 gmol Theoretical mass of CuSO4 (NH4)2 SO4. 6H2O = 0.03 x 397.8165 = 11.9345 g The mass of double salt obtained from the experiment =.

The percentage error = (11.9345-..11.9345) x 100% The percentage yield = (experimental yield theoretical yield) x 100% = (11.9345) x 100% =. ( B ) Preparation of complex salt, Cu(NH3)4 SO4.H2O No. of mole of Cu(NH3)4 SO4. H2O = 0 Relative molecular mass of Cu(NH3)SO4. H2O = 63.54 + 4 [14.0067+ 3(1.008)] + 32.064 + 4(16.00) + 2(1.008) + 16.00 =245.7428 gmol The reaction equation : CuSO4. 5H2O (aq) + 4NH3 (aq) Cu(NH3)4 SO4. H2O (s) + 4H2O

From the equation : 1mole of CuSO4. 5H2O 1mole of Cu(NH3)4 SO4.H2O ::. Theoretical mass of Cu(NH3)4 SO4.H2O = =.g

Mass of complex salt obtained from the experiment =..g

The percentage error = . The percentage yield = ( experimental yield theoretical yield ) x 100% =.

DISCUSSION : In this experiment, when we prepared CuSO4(NH4)2 SO4. 6H2O and Cu(NH3)4 SO4. H2O,we can observe the behaviour between double salt and complex salt and also the difference in their constitution. In part A of the experiment, the double salt CuSO4(NH4)2 SO4. 6H2O is formed when copper sulphate pentahydrate and ammonium sulphate was dissolved in hot water for a several minutes. The color of the solution turn to light blue crystal when the cooling process was done. The color of the solution turn color due to the formation of Cu2+ ions. In order for us to get a perfect and good crystal sample, the cooling down process need to be done slowly. Let the solution cool down for a few minutes before we can get the result.While in part B of the experiment, the complex salt Cu(NH3)4 SO4.H2O was produced when the cupric salt is dissolved in excess ammonia. It will formed a dark blue solution due to the formation of Cu(NH3)4 2+ complex ions. Then the solution was left inside the ice bath for an hour. This steps is important to make sure that the complex ions will form completely. The reason that we used ice bath in this experiment is to help the process of recrystallization occur a lot faster than the usual. The crystal that formed was in dark blue color. The double salt is much more soluble than the complex salt because of the formation of complex ions Cu(NH3)4 2+ in complex salt. From this experiment, the mass of double salt, CuSO4(NH4)2 SO4. 6H2O is .g, which is less than the theoretical value.g. Thus the yield percentage that is obtained is..%. While the mass that we obtained for complex salt, Cu(NH3)4 SO4 . H2O is.g, which is less than the theoretical value,g. Thus the yield percentage that is obtained is.%. While carrying out this experiment there might be some errors occurred that may effects the percentage of yield to be less than the theoretical value. For example when we filtered the salt, we might not do it the right way. There might be a salt that is not well filtered. Besides that, for the complex salt, the salt might not well wash using the ammonia and ether. There are also some problem when we need to take the weight of the salts. The reading of the analytical balance was not stable maybe due to the impurities from the previous experiment that was left inside it. Furthermore, in UV-VIS spectroscopy, for double salt there is no peak occur at 807.39nm with 0.502 absorption. While for complex salt, there is no peak that can be determined.

QUESTIONS : (1) Name three double salt that are important in industry or in laboratory practice. The three double salts are calcium copper chloride [ CuCl2 . 2KCl . 2H2O ], cobalt ammonium sulphate [ CoSO4 (NH4)2 SO4. 6H2O ], ammonium nickel sulphate [ (NH4)2 SO4 NiSO4 . 6H2O ]. (2) Name three other metallic cations that form complex ions with ammonia. Silver (Ag), Nickel (Ni), and Cobalt (Co) (3) When the complex salt is dissolve in water, a slight precipitate is appear. What is this precipitate, and why is it formed ? CuSO4 . 5H2O + 4NH3 + H2O Cu(NH3)4 SO4 . H2O + 5H2O. It is a reversible reaction. Thus, when CuSO4. 5H2O was added to the water, complex ion of Cu ( NH3)4 SO4 . H2O formed. Some of the complex ion is reverse to the CuSO4 . 5H2O salt. So, CuSO4 . 5H2O salt is the precipitate. (4) What is the difference in constitution between tetrammine cupric sulphate and cupric ammonium sulfate? Cu (NH3)4 SO4 . H2O is a complex salt with the elements of ion [ Cu (NH3)4 ] and [ SO4- ] while CuSO4 ( NH4 )2 SO4 . 6H2O is a double salt with the elements of ion Cu, NH4+, SO4, H+ and OH-. Therefore, the difference constitution is [ Cu (NH3 )4 + ] is a complex ion and for double salt, Cu+, NH4+ is a cation.

PRECAUTION STEPS : 1. The complex salts must be rinsed properly with ammonia and ether. 2. Before we do the weighing process, make sure that the crystal are dried completely in the oven. 3. When doing the filteration steps, make sure all the salts are transferred perfectly into the Buchner funnel. 4. Rinse all the apparatus completely with distilled water before we used.

CONCLUSION 1. The mass of double salt, CuSO4 (NH4) SO4. 6H2O obtained isg. While the percentage of yield is..% 2. The mass of complex salt, Cu(NH3)4 SO4 .H2O is g. While the percentage of yield is% 3. The crystal of double salt is light blue colour, whereas the crystal of complex salt is dark blue colour. 4. Double salt is soluble in water, while complex salt is slightly soluble in water REFERENCES