Ellis Greene Section: 4B48 CHM 2046L Unknown Analysis 1 Possible ions 1 I. Cations: Na+, K+, NH4+ 2 II.

Anions: Cl−, NO3−, SO42−, HSO4−, OH− Procedures for the Unknown Analysis: i. Prepare the “neutral water” by: -Adding a counted number of drops of deionized water to a clean testtube. Treat with 1-2 drops of HBtB. Should be yellow. Add tap water, and count the number of basic tap water needed to produce a green color, indicating a pH of 7.0. The ratio of deionized water/tap water will give you “neutral water.” ii. Clean glassware and crucible, etc. iii. Get some indicators, reagents (using your plastic bottles) and litmus papers that you need use during the unknown analysis; iv. Get a unknown card from the stockroom and fill in the necessary information; v. Bring the card to the stockroom and get two unknown samples; vi. Return the unknown card to the personnel in the stockroom when finished. 1. Describe Sample: Phase, color, odor, crystal shape if crystalline, etc. 2. Test on original sample i) Flame test (adhere solids using deionized water) Bushy yellow orange: Na+ (K+ and NH4+ possible) Purple: K+ (No Na+ but NH4+ maybe) No color: NH4+ (No Na+ and K+) ii) NH4+ test a) Place a small portion of original unknown sample in a test tube or spot plate, then add a few drop of 1M NaOH solution, at then same time suspend a red litmus paper (before using it, rinse it with deionized water) over the unknown solution. If red litmus paper turns blue, it indicates the existence of NH4+ ion. OR: b) Place a small portion of original unknown sample in an open crucible, then heating it up, if continuous gray fumes and smoke are discharged, it means you have NH 4+ ion. (Be careful, if you only see a little bit of green or yellow fumes come out, it is due to the moisture of your sample, not from NH4+). 3. Test pH

Using a small portion of unknown sample to make a solution with neutral water, and then test pH with indicators. pH: pH: pH: pH: ~2: HSO4− (No OH−) ~5-6.0: NH4+ ~7: Cl−, NO3−, SO42−, K+, Na+ ≥13: OH− (No HSO4−, NH4+)

4. Make solution Dissolve ½ of unknown sample with 10~15mL deionized water. 5. Specific Ion Tests i) K+ NH4+ present: Place a small portion of unknown sample in an open crucible. Heat the crucible strongly until fumes and smoke are no longer discharged. First allow the crucible to cool down, and then dissolve any residue with no more than 1~2mL deionized water. Now, put 1 mL of this solution in a small vial or test tube, or in a spot plate, then add 2 drops of 6M HAc and 4~6 drops of sodium cobaltinitrite reagent (Na3Co(NO2)6). If yellow precipitates are formed, K+ ion presents. NH4+ is not present: If there is no NH4+ ion, just put 1~2mL of the unknown sample in a small vial or test tube, or in a spot plate, then add 2 drops of 6M HAc and 4~6 drops of sodium cobaltinitrite reagent (Na3Co(NO2)6). If yellow precipitates are formed, K+ ion presents. ii) Cl− Acidify unknown sample solution with 6M HNO3 (stir the solution before you use the blue litmus paper to test its acidity). Adding few drops of 0.02M AgNO3. If white precipitate formed, then Cl − presented. iii) SO42− Acidify unknown sample solution with 6M HNO3 (stir the solution before you use the blue litmus paper to test its acidity). Adding few drops of Ba(NO 3)2 . If white precipitate formed, then SO 42− presented. iv) NO3− Place a single crystal of Fe(H2O)6(NH4)2(SO4)2 in the hollow of a spot plate, then cover the crystal with few drops of the unknown solution, and immediately add two drops of 18M H 2SO4 . If crystal turns brown, then NO3− presented v) HSO4−, OH−

Tested before (Notes: if you get HSO4− ion, then just write down HSO4− (SO42−) because so far we have not any method to decide whether we have SO42− ion or not if HSO4− ion is presented).