A-level Applied Science/Finding out about substances/Qualitative

The basic question addressed by qualitative analysis is: Is there any X in the sample? In contrast, quantitative analysis answers the question: How much X is there in the sample? In practice, qualitative analysis records if the amount of X is above a certain threshold value. Uses of qualitative analysis Reagent Effects 6M HCl Increases [H+] Increases [Cl-] Decreases [OH-] Dissolves insoluble carbonates, chromates, hydroxides, some sulfates Destroys hydroxo and NH3 complexes Precipitates insoluble chlorides 6M HNO3 Increases [H+] Decreases [OH-] Dissolves insoluble carbonates, chromates, and hydroxides Dissolves insoluble sulfides by oxidizing sulfide ion Destroys hydroxo and ammonia complexes Good oxidizing agent when hot 6 M NaOH Increases [OH-] Decreases [H+] Forms hydroxo complexes Precipitates insoluble hydroxides 6M NH3 Increases [NH3] Increases [OH-] Decreases [H+] Precipitates insoluble hydroxides Forms NH3 complexes Forms a basic buffer with NH4+ Limitations Group I: Ag+, Hg22+, Pb2+ Precipitated in 1 M HCl Group II: Bi3+, Cd2+, Cu2+, Hg2+, (Pb2+), Sb3+ and Sb5+, Sn2+ and Sn4+ Precipitated in 0.1 M H2S solution at pH 0.5 Group III: Al3+, (Cd2+), Co2+, Cr3+, Fe2+ and Fe3+, Mn2+, Ni2+, Zn2+ Precipitated in 0.1 M H2S solution at pH 9 Group IV: Ba2+, Ca2+, K+, Mg2+, Na+, NH4+ Ba2+, Ca2+, and Mg2+ are precipitated in 0.2 M (NH4)2CO3 solution at pH 10; the other ions are soluble Many reagents are used in qualitative analysis, but only a few are involved in nearly every group procedure. The four most commonly used reagents are 6M HCl, 6M HNO3, 6M NaOH, 6M NH3. Understanding the uses of the reagents is helpful when planning an analysis. Sample preparation Standard procedures Analysis of mine water sample A. Cations To a 2 cm³ mine water sample: Add sodium hydroxide solution dropwise until it is in excess. Filter the mixture from (1) and add sulphuric acid dropwise to the filtrate. Add aqueous ammonia solution to the acidified filtrate from (2). To a 2 cm³ mine water sample: Add aqueous ammonia solution dropwise until it is in excess. Filter the mixture from (4) and add sulphuric acid dropwise to the filtrate. To a drop of mine water sample: Add a drop of potassium thiocyanate solution. To a drop of mine water sample: Add a drop of potassium hexacyanoferrate (III) solution. Flame test the mine water sample. B. Anions Test the pH of the mine water sample. What anions would react to form gases at this pH? To a drop of mine water sample: Add a drop of barium nitrate solution. To a drop of mine water sample: Add a drop of silver nitrate solution. To a 1 cm³ mine water sample: Add powdered Al and aqueous NaOH – if a reaction occurs test gas with damp red litmus paper. Questions Which ions have you identified as being present? Which ions are definitely not present? Are there any ions which you are unsure about? Write a report of this practical work. Discuss the limitations of qualitative analysis. Give a full account of all your experiments and observations. Risk evaluations Observations Interpretation, explanation and evaluation