Qualitative analytical chemistry I experiments

Qualitative Analysis of The Group I Cations

Wimbo triono 3315081900

University of Jakarta

I. Purpose 1. Separating the group I cations from sample 2. Indentifying the group I cations use specific reagent 3. Knowing chemical properties of group I cations

II. Basic of theory In the classical qualitative analysis scheme, the first ion which are determined are Ag+, Pb2+, and Hg22+. Of all the commons cations, only these form insoluble chlorides under acidic conditions. These cations comprise Group I in the scheme and are separated from general salt solution by precipitation of their chlorides at a pH of about zero. The chloride precipitate is then analyzed the possible presence of silver, lead and mercury (I) on the basic of the characteristic properties of those cations. Silver has only a few water soluble salts, of which the nitrate is certainly the most common. Most of the insoluble silver salts dissolve in cold 6 M HNO3, the main exceptions being the silver halides, AgSCN and Ag2S. Silver ion forms many stable complexes; of these, the best known is probably the Ag(NH3)2+ ion. This comlex is sufficiently stable to be produce when AgCl or AgSCN is treated with 6 NH3; the reaction which occurs is usefull for dissolving those solids. AgBr and AgI are less soluble than AgCl; AgBr will go into solution in 15 M NH3, but AgI is so insoluble that it will not. The silver Thiosulfate complexe ion, Ag(S2O3)23-, is extremly stable, and is important in photography, where it is formed in the “fixing” reaction in which AgBr is removed from the developed negative. Lead nitrate and acetate are the only well known soluble lead salts. Lead chloride is not nearly as insoluble in water as are the chlorides of silver and mercury (I), and becomes moderately soluble if the water is heated. PbSO4 is ion of the relatively few insoluble sulfates. Lead forms a stable hydroxide complex ion and a weak chloride complex. Although lead ordinarily has an oxidation number of +2, there are some Pb (IV) compounds, of which thenist cinnib us PbO2 (brown), this compound is insoluble in most reagents, but will dissolve in 6 M HNO3 to which some H2O2 has been added.

Mercury (I) has only one soluble salt, the nitrate, and even with this compound, excess HNO3 must be present to keep basic Hg(I) salts from precipitating. The Hg(I) ion, sometimes called mercurous ion, is relatively unstable, it will slowly oxidize to Hg(II) if exposed to air, and can be reduced to the metal by reducing cations (e.g. Sn2+). In the presence of species that reaction to Hg (solid, black) and the Hg(II) compound. Mercury(I) chloride has a very characteristic raction with amonia: Hg2Cl2(s) + 2 NH3(aq) -> Hg(s) + HgNH2Cl(s) + NH4+(aq) + Cl-(aq)

III. Instruments and materials • Instruments
1. Pipete

* Material 1. HCl 2. NH4OH 3. Aquaregia

2. Beaker glass
3. Semimicro test tube

4. Centrifuge tube 5. Filter paper 6. funnel

IV. Procedure
1. To 3 ml of sample in a test tube, add 0,5 ml 6 M HCl. Stir well and

centrifuge. Decant the liquid, into a test tube. To make sure precipitation of group I cations was complete, add 1 drop of 6 M HCl to the liquid. Wash the precipitate with 2 ml water and 3 drops of 6 M HCl. Stir well sentrifuge and discard the wash liquid. Wash the precipitate again with water and HCl, centrifuge and discard the wash.
2. To the precipitate from step 1, which contains the chlorides of

the group I cations, add about 4 ml water. Heat in the boliling water bath for at least three minutes, stirring constantly, centrifuge quickly and decant the liquid, which may contains Pb2+, in test tube
3. Confimation of the presence of lead. To the liquid from step 2

add 2 drops of 6 M acetic acid and 3 or 4 drops of 1 M K2CrO4.

The formation of a yellow precipitate confirms the presence of lead. Centrifuging out the solid may help with the identification, because the liqiod phase is orange.
4. Confirmation of the presence of mercury. If lead is present, wash

the precipitate from step 2 with 6 ml water in the boiling water bath. Centrifuge and test the liquid for Pb2+. Continue the washings until no positive reaction to the lead test is obtained. To the washed precipitate add 2 ml 6 M NH3 and stir well. A black or dark gray precipitate estabilish the presence of the mercury (I) ion. Centrifuge and decant the liquid, which may contain Ag(NH3)2+, into test tube. Identifiying filtrat for Ag ion.

V. Data of experiments sample Sample+HCL Precipitate + Hot water Filtrate + K2CrO4 …………+ NaOH Precipitate + NH4OH Filtrate + KI …………+ NaOH …………+ K2CrO4 Precipitate + Aquaregia Filtrate + KI ………..+ NaOH Experiments result A white precipitate Half of precipitate solute An yellow precipitate Precipitate soluble A gray precipitate A green precipitate Precipitate soluble An orange precipitate A white precipitate A red precipitate A white precipitate

VI. Analysis of data

Sample that will identifying compose liquid and unknown precipitate. So, precipitate in sample have to dissolved berfore identification. Assume that dissolving used H2O will cause precipitation of phosphate of group III, IV cations and magnesium, dissolving sample used HNO3. The unknown precipitate had dissolved. HCl 6 M add into sample. A white percipitate formed and establish the presence of group I cations. Chlorides from other cations will dissolve, except group I cations. Centrifuge and decant the liquid into test tube. Ag+ + Pb2+ + Hg22+ -> AgCl(S) + PbCl2(s) + Hg2Cl2(s) Precipitate which may contains Pb2+, Ag+ and Hg(I) wash with hot water. PbCl2 which soluble in hot water will dissolve. The wash liquid use for identification of Pb2+. The wash liquid divide into two test tube. K2CrO4 added into first test tube, a yellow precipitate indicates the presence of Pb2+. The second test tube added NaOH excess, no precipitate result from these because Pb2+ will be complex ions with hidroxide. PbCl2(s) -> PbCl2(Aq) PbCl2(aq) + K2CrO4 -> PbCrO4(s) + 2KCl

The precipitate from separating Pb2+ added NH4OH in order to separate AgCl from Hg2Cl2. AgCl dissolve in NH4OH excess form ion complex while Hg(I) form precipitate of Hg and Hg(NH2)Cl. A white precipitate which slowly become gray indicates the presence of Hg(I). AgCl + NH3 -> [Ag(NH3)2]+ + ClHg2Cl2 + NH3 -> Hg(s) + Hg(NH2)Cl(s) + NH4+ + ClCentrifuge and decant the liquid into a test tube. To confim the presence of mercury, precipitate dissolved in aquaregia. The gray precipitate become white because of Hg dissolve in HNO3 but Hg(NH2)Cl not. A white precipitate indicates Hg(NH2)Cl. The liquid added KI to make a red precipitate, from experiments red precipitate formed and establish the presence of mercury in the sample.

Liquid from separating AgCl from Hg2Cl2 used to identify Ag+ in sample. Based on experiments, the presence of Ag+ in sample cannot be sure because the experiments results are different with theory.

VII.

Task Write chemical equations for each step • HCL 6 m Ag+ + Pb2+ + Hg22+ -> AgCl(S) + PbCl2(s) + Hg2Cl2(s) • Hot water PbCl2(s) -> PbCl2(Aq)

K2CrO4 PbCl2(aq) + K2CrO4 -> PbCrO4(s) + 2KCl

NaOH PbCl2 + 2NaOH -> Pb(OH)2(s) + NaCl .............+ 2NaOH excess -> Na2[Pb(OH)4]

NH3 AgCl + NH3 -> [Ag(NH3)2]+ + ClHg2Cl2 + NH3 -> Hg(s) + Hg(NH2)Cl(s) + NH4+ + Cl-

HNO3 6Hg(s) + 8HNO3 -> Hg22+ + 2NO + 6NO3- + 4H2O

VIII.

Conclusion 1. The Group I cations is presence in the sample
2. PbCl2 dissolve in hot water, but AgCl and Hg2Cl2 cannot 3. Identify Pb2+ use K2CrO4 and NaOH establish the presence of

Pb2+ in the sample

4. Identify Hg22+ use NH3 establish the presence of Hg22+ in

sample 5. Sample contains lead and mercury

IX. Bibliography

Darsati, Siti, dkk. 1999. Dasar-Dasar Kimia Analitik. Bandung: FMIPA UNJ Haryadi, W. 1990. Ilmu Kimia Analitik Dasar. Jakarta: Gramedia Khopkar, SM. 1990. Konsep Dasar Kimia Analitik. Jakarta: UI Press Oktaviani, Isnania, P. 2008. Laporan Praktikum KA I. Jakarta: UNJ Vogel. 1979. Analisis Anorganik Kualitatif Makro dan Semimikro. Jakarta.: PT Kalman Media Pustaka

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