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

SO42-, OH-, CO3-, HCO3Tests pf the Solid Sample 1. Flame Test: a. If the flame appears Bright Orange: Na+ present, K+, NH4+, Ca2+, Al, Mg to be determined b. If the flame is bright red: Ca+ present, Na+ not present, K+, NH4+, Al, Mg to be determined c. If the flame appears Purple: K+ present, no Na+ Ca+, NH4+, Al, Mg to be determined d. If the flame has no change, NH4+, Al, Mg may be present, no Na+, no K+ Ca2+ 2. Test for NH4+ a. Add OH- and add heat to convert to NH3 b. Put damp red litmus paper above to see if any color change occurs c. If there is an NH3 odor, NH4+ is present. If the litmus paper turns blue, NH4+ is present Solution Preparation d. Use 1/3 to of the sample and dissolve in 15mL of deionized H2O e. Only use 1-2mL of the unknown solution for each test 3. Solution pH a. First use pH paper (wet with deionized H2O) and then use indicators; start with HBtB and go from there based on color and the pH indicator chart b. Determine pH i. NH4+: pH 5, no OH-, no HSO4ii. OH-: pH 13, no NH4+, no HSO4iii. HSO4-: pH 2, no OH-, no NH4+, SO42- cant be determined iv. SO42-: pH~d.i H2O 7.5, no ions present which can affect the pH c. pH equations i. NH4+ + H2O NH3+ + H3O+ ii. NH3 + H2O NH4+ + OH- (there is no NH3 in the unknown) iii. SO42- + H2O HO- + HSO4iv. HSO4- + H2O H3O+ + SO424. Test fpr 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 (make sure pH ~1) 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 Na(NO3)2 to 10-20 drops of the solution. If ppt forms then HSO4- or SO42- is be present. To distinguish between the two, take a look at the pH of your original solution. 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 a 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, a brown solution will appear 8. Removal of NH4+ if present a. Heat a pea-sized amount of the sample in a crucible b. Re-dissolve the obtained residue in 10 drops of d.i water, and test for K+ 9. K+ test (Cobaltinitrate Test) a. Add one drop of 6M HAc and 2-3 drops of the cobaltinitrate reagent to 10-15 drops of the sample solution. Using pH paper, check to see if the pH is about four due to a color change to orange. b. If yellow ppt forms- K+ present i. Potassium and ammonium solutions each form a precipitate, showing that they are in the presence of sodium 10. Test for CA2+ a. Add excess Na2CO3 to solution b. If white couldy ppt forms, Ca2+ is present 11. 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 for later

f. Add excess 2M NaOH to the ppt i. If it completely dissolves, Ag+ is present ii. If it doesnt completely dissolve, Mg2+ is present iii. If it doesnt completely dissolve, centrifuge again g. At saturated NH4Cl to liquid h. If a ppt forms, Al3+ is also present 12. Non-soluble salt test a. Insoluble Ion b. Ca(OH)2 c. CaCO3 d. CaSO4x2H2O e. MgCO3 f. Mg(OH)2 +1M HCl Flame Test Soluble Orange Soluble+bubbles Orange Insoluble Soluble+bubbles No change Soluble No change