Unknown Lab 5 Cations: Na+, K+, NH4+, Ca2+, Al3+, Mg+2 Anions: HSO4-, Cl-, NO3-, SO42-, OH-,

CO32-, HCO31) Flame Test: a. If flame appears Bright Orange: Na+ present, K+, NH4+, Ca2+, Al, Mg to be determined. b. If the flame is bright red: Ca2+ present, Na+ not present c. If the flame is Purple: K+ present, no Na+, no Ca2+ d. If the flame has no change, NH4+, Al, Mg may be present, no Na+, no K+, no Ca2+ 2) Test for NH4+ a. Put some of the sample into a vial and add some drops of 6M NaOH b. Put damp red litmus paper above to see any color change c. If there is an NH3 odor, NH4+ is present. If litmus paper turns blue NH4+ is present Solution Preparation 3) Solution pH Use sample and dissolve in deionized water Use 1-2 mL for each test a. First use pH paper and then use indicators, start with HBtB b. Determine pH 1. NH4+:pH 5, no OH-, no HSO42. OH-: pH13, no NH4+, no HSO43. HSO4-: pH 2, no OH-, no NH4+, SO42- cant be determined 4. SO42-: pH 7.5, no ions present which affect pH c. pH equations 1. NH4+ + H2O <-> NH3+ + H3O+ 2. NH3 + H2O <-> NH4+ + OH- (no NH3 in the unknown) 3. SO42- + H2O <-> HO- + HSO44. HSO4- + H2O <-> H3O+ + SO424) Test for HCO32- and CO3a. Add 2 M HCl to see if solid solution bubbles b. If pH is 8-9, HCO2- is present c. If pH is 10-12, CO32- is present 5) Test for Cla. Make the solution acidic by adding 1 M HNO3 until the blue litmus paper turns red b. Treat with 0.02M AgNO3 c. If a precipitate forms, Cl- is present. It should be very white and cloudy 6) Test for SO42- and HSO4a. Make the solution acidic by adding 1M HNO3. Add .25M Ba(NO3)2 to 10-20 drops of the solution. If ppt forms then HSO4- or SO42- is present. Check pH to determine b. Use indicators to determine the pH of the sample. If the HNV indicator turns blue with a pH of 2 it may be HSO4-. If the HBTB turns blue-green with a pH of 7.5 it may be SO42-. If HSO4- and SO42- are combined at an equal concentration, the pH lowers to 1. c. If HSO4- is found, SO42- will be noted as present. 7) Test for NO3a. Place a small amount of Fe(OH2)6(NH4)2(SO4)2 in a spot plate b. Cover it with the sample solution c. Immediately add two drops of 18M H2SO4 d. If NO3- is present, brown solution will appear

8) Removal of NH4 if present a. Heat small amount of sample in crucible b. Re-dissolve the obtained in 10 drops deionized water and test for k+ 9) K+ test (Cobaltinitrate Test) a. Add one drop of 6M HAc and 2-3 drops of the cobaltinitrate to 10-15 drops of the sample solution. Using pH paper, check to see if the pH is 4 b. If yellow ppt forms K+ present 10) [Separation] and Test for CA2+ a. Add excess Na2CO3 to solution b. If cloudy ppt forms, Ca2+ present, centrifuge and repeat to separate Ca2+ out 11) [Separation] and Test for Mg2+ and Al3+ a. Place sample of solution in test tube b. Add excess 6M NH3 c. If ppt forms, one or both are present d. Separate using centrifuge e. Decant liquid and save f. Add excess 2M NAOH to ppt 1. If completely dissolves, Al3+ present 2. If it doesnt completely dissolve, Mg2+ is present and recentrifuge g. Add saturated NH4Cl to liquid h. If a ppt forms, Al3+ is present 12) Non-soluble salt test Insoluble Ion +1M HCl Flame Test pH a. Ca(OH) 2 Soluble Orange 12.5 b. CaCO3 Soluble + Bubbles Orange 10 c. CaSO4x2H2O Insoluble 7 d. MgCO3 Soluble + Bubble No change 9.5 e. Mg(OH)2 Soluble No Change 10.5 Alums: Na[Al(H2O)6](SO4)2*6H2O, K[Al(H2O)6](SO4)2*6H2O, NH4[Al(H20)6](SO4) 2*6H2O