Introduction Cations that are mixed in an aqueous solution can be separated by selective precipitation.

It is done by adding reagents which contains the anions required to precipitate one or more cations in the mixture (Zumdahl, 2010). Selective precipitation is ensured when the Qsp value of the more soluble compound is almost equal to its Ksp. It also makes certain that the Ksp value of the less soluble compound is outdone (Silberberg, 2006). Ions in a mixture can be identified by qualitative analysis. The analysis requires the cations to be separated in five major groups: 1. Insoluble chlorides; 2. Acid-insoluble sulfides; 3. Base-insoluble sulfides and hydroxides; 4. Insoluble phosphates; and 5. Alkali metal and ammonium ions. Different schemes are devised to separate this ion groups such as flame test and precipitation reaction. There are several types of reactions that are used in qualitative analysis. Acid-base reactions is one of the most popular in the quantitative analysis. Acid, as defined by Bronsted and Lowry, is a proton donor while the base is an proton acceptor. When the ion product (Qsp) is greater than the solubility product principle (Ksp) precipitate is formed and this is called as precipitation reaction. This kind of reaction also is widely used in qualitative analysis. Addition to that, oxidation-reduction reactions and disproportionation (auto ionization) reactions are considered during a separation of ions. Formation of complex ions are also favored in qualitative analysis. Complex ions are formed when a “central metal cation is bonded to form two up to six lone pairs of electrons on surrounding ligands”. Ligands are the molecules that can donate one or more lone pairs of electrons. The objectives of this exercise were: The experiments were performed in the Room 105 Wing B of the Institute of Chemistry in the University of The Philippines Los Banos on February 22, 2012.

Materials Reagents Concentrated HNO3 6M HCl 6M NH3 Acetic acid K4fe(CN)6 1% dimethylgyoxime (DMG) 6M CH3COOH Solid Na2S2O3 Na2HPO4 6M NaOH 0.2M Na2S Apparatus Hot plate Stirring rod Dropper Centrifuge tubes centrifuge Iitmus paper watch glass evaporating dish hot water bath Pasteur pipe

five drops of 0.1M k4fe(cn)6 wad also added. the tube was centrifuged.Procedure For the determination of the presence of group d cations. 1% Dimethylglyoxime was added also in the solution. a solution contining the cations was gathered by the group and label it as cd1. 6M NH3 was added to the solution until neutral then it was made slightly acidic by adding 2 drops of of 6M acetic acid. While on the other tube. The addition of nitric acid produced the oxides of the cations and stayed solid in the solution.1m of k4f3(cn)6 was also added.3 grams of Na2S2O3 was added. ammonia and oxalate from the previous analyses must be removed by heating the solution to dryness. The reactions were represented by the chemical equations: . 2 drops of 6M acetic acid was added to one of the tubes to make the solution slightly acidic and then. Also. 8 drops of 0. The results were then recorded. 6M acetic acid was added to the centrifugate until it was slightly acidic then. 6 drops of 6M HCl was then added and the solution was stirred and centrifuged. the supernatant was complete decanted in a tube. The precipitate was discarded. After standing. The supernatant was quickly decanted in a tube. The precipitate was washed twice with distilled water.2M Na2S was added. For the centrifugate of the remainder of CD1. The ammonium ions were present and the following reaction occur: The oxalate present in the sample decomposed and it produced co2 gas. Concentrated hno3 was added and was heated to dryness. 6M NH3 was added to the remainder of cd1 until neutral and 2 drops of 6M CH3COOH was added to the solution also to make it slightly acidic. 4 drops 0. Data Results and Discussion For the determination of the group D cations. five drops of 0.1M Na2HPO4 was added to the tube and it was allowed to stand for few minutes. 6M NH3 was added to it. Then. 0. For the precipitate of the remainder of CD1. 50 drops of 6M NaOH was added then the solution was stirred and centrifuged. Another drop of CD1 was obtained and again. 6 drops of the centrifugate was obtained and each three drops was put in separate tubes. 6M NH3 was added to each of the tubes until it was neutral. The solution was heated for 10 minutes in a hot water bath. 4 drops of K4Fe(CN)6 were added to the solution. The tube was then cooled and centrifuged. 6M NH3 was added to the solution until basic. The reaction was observed and recorded. Then. The chemical reaction was: It is important to remove the traces of ammonia and oxalate in the solution for it could interfere in the determination of the group d cations.

which was characterized by the white precipitate confirmed the presence of mg2+ in the test solution. The solution was made slightly basic in order the precipitate formed. zn. ni and cd as sulfides. The reaction was represented by: As shown in cd1b. The net ionic disproportionation reaction was shown: The free sulfide ions reacted with the cations. cu. mg nh4po4. For the further confirmation of the presence of mg2+ cations. The dmg must be deprotonated before it reacts with Ni2+ ion. This was done by precipitating the zn. The reaction produced a black precipitate. The purpose of adding ch3cooh was for the test solution to be made slightly acidic to prevent the formation of hydrogen cyanide. This was done to liberate the group d cations that were dissolved in an aqueous solution. The reaction involved was: The ammonium ions and hydrogen phosphate ions reacted with the magnesium ions in the solution. (equation) The solution was now tested for the presence of Cu2+. the test solution was made neutral by nh3 and slightly acidic by the addition of ch3cooh. The Ni2+ ions form a highly colored precipitate with dimethylgloxime ions only. This poisonous gas was produced when the hexacyanoferrate was added in a strongly acidic solution. By the application of heat and the slightly acidic solution. In CD1a. . The solution was made slightly basic with aqueous ammonia. The test solution was made slightly acidic by the addition of ch3cooh. The deprotonating of dmg with ammonia was shown in the equation: The deprotonated dmg reacted with the free ni2+ ions and produced nickel dimethylglyoxime complex. It produced a cherry red solution that confirmed the presence of ni2+ ions. nh3 and 1% dmg was added to the test solution. sodium thiosulfate dissociated. ni and cd cations. ni and cd sulfides were insoluble while the magnesium ions did not formed a sulfide. Hexacyanoferrate was then added. The supernatant was blue because of the unreacted cu. The addition of hexacyanoferrate in the solution formed a precipitate for it reacted to copper to form copper hexacyanoferrate which was maroon in color as its distinct appearance. thus the magnesium ion remained in the solution and did not precipitate. for the confirmation of the presence of cu2+. The separation of group d cations was needed to confirm the presence of mg2+. cu. Zn2+ and Cd2+. as shown in the table (CD2). as shown in the table. nh3. Mg2+. The sulfide ions were provided by sodium thiosulfate.6M HCl was added to dissolve the oxides. nh3 and na2hpo4 was added to the solution. ch3cooh and na2so3 were added in the solution and heat was applied. which was characterized by a cherry red precipitate. It was shown in the equation: The product formed. The resulting precipitate and supernatant liquid was maroon in color. The reaction was as followed: In the remainder of Cd1. The color of the precipitate of the zn and cd were masked by the blackness of the precipitate of ni and cu. Ni2+. The chemical equations and the characteristic colors were shown below: The zn.

two ways was used. zn2fe(cn)6 was formed and it was characterized as white precipitate. 12M HCl and k4fe(cn)6 was added. 6m hcl was added. k3fe(cn)6 was used as an indicator. The product formed was from the reaction of hydroxide ions with the zinc sulfide in the solution. If the ions were really absent or insufficient. By the addition of na2s. which is a yellow precipitate. The second pattern to confirm the presence of cadmium ions in the solution was by adding nh3 and na2s. in pd2. the desired color of the precipitate was not obtained. A pink precipitate was observed.2M Na2s were added to other tube with three drops of cd4. The errors in the experiment may be attributed in the absence or insufficiency of cadmium ions present in the solution. naoh was added in the solution. it produced a pink precipitate. The reaction was shown below: For the confirmation of the presences of zinc2+ in the solution k4fe(cn|)6 was used.1. The reaction was shown: In cd3. The precipitate can be determined if it is zinc or cadmium ions by means of sulfide precipitation. (equation) However. (equation) After the confirmation of zinc2+. The first way to confirm the presence of the cadmium ions. This is done to favored the reaction that favors the formation of the confirmatory compounds of zinc and cadmium. After the addition of k4fe(cn)6. The result of the experiment was attributed in some errors. This was done to liberate the zinc ions in the form of tetrahydroxozincate complex. (equations) . Nh3. The presence of cu2+ produced pink precipitate that was manifested in the experiment. no precipitate was formed. Instead. precipitation would not be observed. Acid was dropped on the the zinc ions and cadmiums ions in the test solution before adding k4fe(cn)6. the desired yellow precipitate was not seen. White precipitate was observed after the addition. Nh3 and 0. The addition of acid liberates the zinc2+ from its hydroxide (tetrahydroxozincate complex in pd1). Zinc ions will not form any colored precipitate with sulfide ions while cadmium will react to sulfides forming CdS. in the portion of pd1.In table 1. The addition of acid liberated mostly the cadmium ions from its sulfide while the nis and cus remained insoluble in their sulfides. Cd2fe(cn)6 was the product of the reaction of cd2+ ions and k4fe(cn)6 and was characterized by white precipitate. The zinc and cadmium ions formed both white precipitates when reacting with k4fe(cn)6. The reaction of cadmium ions with the acid was represented in the equation: For the confirmation of cadmium ions in the solution. No precipitate was observed. cds was the product of the reaction of cd2+ ions and na2s and was seen as yellow precipitate: (equation) Yet. cd2fe(cn)6 and zn2fe(cn)6. ch3cooh and k4fe(cn)6 was added to the tube with three drops of cd4. Dissolution of some precipitate had taken place while some black precipitate remained. One possible explanation was that the cu2+ ions were not completely eliminated before the test for the presence of cd2+ ions.

The solution must be acidic to liberate most of the ions that were in a compound and also to prevent the evolution of toxic gases. . Results showed that the formation of maroon precipitate after adding k4fe(cn) to the test solution confirmed the presence of copper ions. In the experiment on the quantitative analysis of group d cations. Oxidation-reduction reactions were also needed to reduced or oxidized some ions in order to react with other reagents. thus errors in the experiment were considered. For the verification of cadmium presence in the test solution. na2s was added but no precipitate was formed. Also. It was also recommended that the ph of the test solution should be monitored for the results not to be flawed. two ways of precipitation were observed. reagents that contains the anions needed to precipitate the cations were obtained. it can be established that the ph of the solution was crucial in seperating the cations. (equation) Conclusion For the confirmation of the presence of group d cations namely: ….The less favorable reaction by the addition of acid was the formation of the toxic gas. the presence of nickel ion was established upon addition of dimethylgyoxime and cherry red precipitate was formed. However. A portion of the test solution was subjected in k4fe9cn)6 and a pink precipitate was produced. some solution must be basic in order to deprotonate some reagents thus permitting the occurrence of confirmatory reactions. The formation of a specific complex ion gave characteristic color thus increasing the possibility of accurate confirmation of ions. it was recommended to use other reagents for the precipitation reactions. Moreover. HCN. a white precipitate. For further study. The results were invalid. the different principles in separation of the cations were very important. In the other portion of the solution. It was concluded that understanding the effect of the ph and principles of separation of ions were essential in quantitative analysis. Addition of sodium hydrogen phosphate confirmed the presence of magnesium ions by forming a white precipitate while the addition of k4fe(cn)6 confirmed the presence of zinc ions by forming also.

Sign up to vote on this title
UsefulNot useful