Jason Howell

Section: 0750
Unknown Lab 1 Scheme
I.
II.

III.

Possible ions: Na+, K+, H4N+, HO-, Cl-, NO3-,SO42- . Examine unknown
samples to see if they are either compounds or pure substances.
Test on Original Sample
i. Flame Test
Use wire loop dipped in DIW to adhere the unknown substances to the
wire to examine flame color. After each use, wash wire with HNO3
followed by DIW. Repeat for each substance.
ii. Test for H4N+
In Parallel, add 5mL of NaOH to a small amount of each unknown
substance. Then suspend red litmus paper over the solution to detect if any
NH3 gas is being formed.
Solution Test
i. Dissolve Unknowns
Dissolve about to 2/3s of sample into 10-15 mL DIW. Also prepare
Neutral water for pH testing with indicators.
ii.

Determine pH of Samples (HSO4-/ OH-)

Dissolve a small amount of each sample into NEUTRAL WATER not DIW
and determine the pH by starting at the indicator Bromthymol blue. If pH is
lower than 3 then HSO4- will be present in the solution. A pH of around 13
will indicate that OH- will be present in the solution.

iii.

Test for Cl- by Precipitation

Add 1M HNO3 drop wise until each solution is acidic before adding one
drop of 0.02 M AgNO3 to each. Test solution for acidity by touching small
amounts of solution to blue litmus paper.

iv.

Test for SO4Add 1M HNO3 drop wise until each solution is acidic before adding one of
0.25M Ba(NO3)2 to each. Test solution for acidity by touching small
amounts of solution to blue litmus paper.

v.

Test for NO3In a spot plate, add a crystal of Fe(OH2)6(H4N)2(SO4)2 at the center of the
depression. Cover the crystal with a few drops of test solution. Immediatley
add two drops of 18M H2SO4. Allow H2SO4 to flow without agitation to the
top. If NO3- is present, a brown solution will form on the surface of the
crystal where H2SO4 contacts it.

vi.

Test for K+ and NH4+

Add one drop of 6 M HAc and 2-3 drops of sodium cobaltinitrite to 10-15
drops of both sample dilutions. Observe to see if a precipitate forms.

IV.

Preforming Necessary Separations

i.

Test for K+ in the presence of NH4+

Place small amount of original sample into crucible and heat strongly until
smoking from the crucible ceases. Then proceed with the same
precipitation test for NH4+ and K+.