EXACT SCIENCE DEGREE IN CHEMISTRY LAB - B PRACTICE 3 - IDENTIFICATION cations H +, Na +, K +, Li +, Mg2 + and NH4 + Objectives • Identify cations in a solution

using reactions or physico-chemical sp ecific; understand the operations involved in the test flame; identify the catio ns of alkali metals and ammonia present in aqueous solutions. • General For the purpose of systematic qualitative analysis, the cations are clas sified into five groups, having as its basic peculiarity of certain reagents [1,2,3]. The reagent s used for the classification of most common cations are hydrochloric acid (HCl) , hydrogen sulfide (H2S), ammonium sulfide (NH4S) and ammonium carbonate ((NH4) 2CO3) [1]. The classification is based on how the cations react or not the forma tion of precipitates. Therefore, one can say that the most common classification of ions is based on differences in solubility of their chlorides, sulfates and carbonates. The common cations, which do not react with any of these reagents fo rm a group which includes the magnesium ions, sodium, potassium, ammonium, lithi um and hydrogen. In this case, as there is no specific reagents for these cation s, they are analyzed by specific reactions or physical testing, as the flame tes t. This test involves inserting a sample containing the cation of interest in th e flame of a Bunsen burner. When the atoms of the element receiving energy from the flame is promoting its electrons to higher energy levels. This energy is qua ntized, ie only a specific energy can promote electrons between different energy levels. Thus, when the electron returns to ground state, occurs releasing the s ame amount of energy used for excitation. Since it is quantized it is specific t o a given chemical species, and when the issue occurs it occurs in the visible c olor characteristics and specific [1,4,5]. This phenomenon is used in the prepar ation of fireworks, whose colors are obtained by employing salts of alkali metal s and / or alkaline-earth metals, which when subjected to promoting electronic heat present, then the emission in the visible region, prov iding the spectacle of lights and colors typical of fires. Experiments in soluti on, also called wet, may be useful for identification of these cations, as will be seen below. • Test Procedure Call Dip the platinum wire in hydrochloric acid (HCl), concentrat ed (for cleaning and decontamination), then in substance, so that a sufficient amount of stay adhered to the wire. Bring the wire to the region oxidizing flame and observe the color ation appears. Then record the results in Table 1. Finally do a mixture of 1 mL of sodium with 1 mL of potassium in a test tube and test flame with and without the cobalt glass. Table 1 - Results of the flame test for alkali metals sodium potassium lithium C ation Sodium + potassium (without cobalt glass) sodium + potassium (through the cobalt glass) After each test, the platinum wire should be cleaned by immersing themselves in the same hydrochloric acid (HCl) and applying the flame until no c olor is observed. Coloration of the flame Specific reactions in aqueous (wet) 1) Magnesium a) of disodium hydrogen Mg2 + N H3 + + HPO4-2 → Mg (NH4) PO4 ↓ Add to test tube 2 drops of a solution of Mg (NO3) 2 0.2 mol L-1, 10 drops of water, 2 drops of HCl 6 mol L-1, 3 drops of disodium hi drogenofostato 3 mol L-1, and Finally, slowly add drops of NH4OH 6 mol L-1 to the middle of the solution becom es alkaline. Identify the product and the concepts involved. b) p-nitrobenzene-azo-resorcinol (or magneson I) Add 2 mL vial of test solution [Mg (NO3) 2], slightly acidified with HCl, one drop of reagent and a sufficient

amount of 2 mol L -1 NaOH, to make the solution strongly alkaline (2-3 mL). It i s an excellent confirmatory test in macro analysis, but it is essential to have a blank with reagents that often produce a blue color. The reagent consists of a 0.5% solution of p-nitrobenzene-azo-resorcinol in NaOH 0.2 mol L-1. Identify th e product and the concepts involved. 2) Potassium a) perchloric acid (HClO4) Add 5 drops of KCl 0.2 mol L-1 and 5 dro ps 20% HClO4. Identify the product and the concepts involved. K + + ClO4-KClO4 → ↓ b) hexanitritocobalto (III) Sodium Add 3 drops of KCl 0.2 mol L-1, 3 drops of HA c 3 mol L-1 and NAAC same volume of 3 mol L-1. Add a tip spatula hexanitritocoba lto (III) sodium. Identify the product and the concepts involved.€3K + + [Co (NO2) 6] 3 - → K3 [Co (NO2) 6] ↓ 3) Ammonium a) sodium hydroxide NH4 + + OH-→ NH 3 ↑ + H2O Th e release of ammonia in this reaction by mild heating, can be identified: the od or (CAUTION! THERE IS A TECHNIQUE TO CORRECT THIS TYPE OF TEST. CHECK THE TEAM O F INSTRUCTORS) by the formation of white fumes of ammonium chloride, when a glas s rod moistened with concentrated hydrochloric acid is kept in steam by color change (red to blue) litmus paper Take the tests and identify the product and the concepts involved. Unknown sample: Your group should receive a solution containing at least one of the above cations. Divide the sample into small pieces and perform the tests lea ding to identification of the cation. Enter the result to the teacher. Drafting of the report: Describe all reactions performed in the first part and t he results obtained in both reactions, as in flame tests. Include the report in Table 1. As for the unknown sample, which informs the cation and which identifie d the strategy used for their identification. Reference: 1. A. I. Vogel Qualitative Analytical Chemistry, Trad. A. Gimeno, Mes tre Jou, São Paulo, 1981. 2. N. Bacan, O.E.S. Godinho, L. M. Aleixo, E. Stein Semi microanálise Introduction to Qualitative Research, 7th Edition, Edunicamp, Campina s, 1997. 3. V.N. Qualitative Chemical Semimicroanalysis Alexeyev, Mir, Moscow, 1 980. 4. K.W. Whitten, RE Davis, ML Peck General Chemistry with Qualitative Analy sis, 5th, Saunders, Forth Worth, 1981. 5. F. Okumura, E.T.G. Chevalier, J. A. No brega Quím. Nova, in press.