Unknown Scheme

Possible Ions
I.
Cations
a. Na+, K+, NH4+
II.
Anions
a. Cl-, NO3-, SO42-, HSO4-, OHProcedure
I.
Prepare neutral water by
a. Use DIW in a clean test tube. Treat with 1-2 drops of HBtB. This should be yellow. Add
tap water drop by drop and count how many it takes to produce a pH of 7.0, which should
be green. This will give you the ratio of DIW/tap water for neutral water
b. Clean glassware, crucible, any other instrument
c. Get indicators, reagents, and litmus papers that will be needed during unknown analysis.
d. Get an unknown card from the stockroom and fill in the necessary information
e. Bring the car to the stockroom and retrieve two unknown samples
f. Return the unknown card to the stockroom personnel when finished
1. Describe Sample
a. Phase, color, odor, crystal shape if crystalline
2. Test on Original Sample
a. Flame test:
adhere samples using DIW
i. Bushy Orange Na+ present (possibly K+ and NH4+ present)
ii. Purple K+ (No Na+ but maybe NH4+)
iii. NH4+ (No Na+ or K+)
+
b. NH4 Test
i. Place a small portion of the original unknown sample in a test tube or spot
plate, and then add a few drops of 1M NaOH solution, at the same time
thsuspend a red litmus paper (rinse with DIW) over the unknown solution. If
the red litmus paper turns blue, this indicates the existence of NH 4+ ion because
NH3 is present. If it does not change then:
ii. Place a small portion of original unknown sample in an open crucible, and then
heat up. If continuous gray fumes and smoke are discharged, then you have
NH4+.
c. Test pH
Using a small amount of unknown sample to make a solution with neutral water,
and then test pH with indicators
i. pH: ~ 1.5-2HSO4- (No OH- )
ii. pH: ~2.5 SO42
iii. pH: ~5-6.0 NH4+
iv. pH : ~ 7 Cl-, NO3-, SO42-, Na+, K+
v. pH 13 OH- (No HSO4- or NH4+)
3. Specific Ion Tests
a. K+
i. With NH4+ present:
1. Place a small portion of the 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

more more than 1-2mL of DIW. Now put 1 mL of this solution in a small
vial or test tube, or in a spot plate, and then add 2 drops of 6M HAc and
4-6 drops of sodium cobaltinitrite reagent (Na3Co(NO2)6) If yellow
precipitate forms, then K+is present
ii. Without NH4+ present:
1. Just put 1-2 mL of the unknown sample in a small vial, test tube, or spot
plate. There is no need to heat this. Add 2 drops of 6M HAc and 4-6
drops of sodium cobaltinitrite reagent (Na3Co(NO2)6) If yellow
precipitate forms, then K+is present.
b. Cli. Acidify unknown sample with 6M HNO3 (stir the solution before you use the
blue litmus paper to test its acidity). Add a few drops of AgNO 3. If a white
precipitate forms, then Cl- is present
c. SO42i. Acidify unknown sample with 6M HNO3 (stir the solution before you use the
blue litmus paper to test its acidity). Add a few drops of Ba(NO 3)2. If a white
precipitate forms, then SO42- is present
d. NO3i. Place a single crystal of Fe(H2O)6(NH4)2(SO4)2 in a spot plate, then cover the
crystal with a few drops of the unknown solution, and immediate add two
drops of 18M H2SO4. If the crystal turns brown, then NO3- is present.
e. HSO4 VS. OHi. Use the pH to test for HSO41. If a pH of ~1.5, then HSO4ii. Use the pH to test for OH
1. If pH 13, then OH-