Instruction for unknown 9A/9B

Possible ions:
1. Cations: Na+, K+, NH4+, Ca2+, Mg(OH2)62+, Al(OH2)63+Zn(OH2)62+, Ag(OH2)2+,Cu(OH2)62+
2. Anions: HO-, CO32-, HCO3-, SO42-, HSO4-, NO3-, Cl-, HS-, O2-
3. Possible insoluble substance: Ca(OH)2, CaSO4•2H2O, CaCO3, MgCO3, Mg(OH)2AgCl, Ag2O,
Ag2CO3, Ag2S, Ag2SO4, ZnS, Zn(OH)2, CuO, CuS, CuCO3
4. Alums

Notes:
--9A (the sample with the numerical label) is a pure salt, which means it only contains
two (one cation and one anion) or three (alums, i.e., two cations and SO42−) ions.
--The insoluble substance could be one or more kinds of the above compounds.
They will not issue Zn(OH)2/ ZnS in the same sample, nor would a MgCO3/ Mg(OH)2
be issued.
Possible Ions
i) Cations: Na+, K+, NH4+, Ca2+, Mg(H2O)62+, Al(H2O)63+
ii) Anions: Cl−, NO3−, SO42-, HSO4-, OH−, CO32-, HCO3−
iii) Possible INSOLUBLE compounds: Ca(OH)2, CaSO4•2H2O, CaCO3, MgCO3, Mg(OH)2

1) Flame Test
* Use pea-sized solid + 5 drops 1M HNO3 (stir!) – Watch out for
bubbles!*

Intense yellow: Na+ (K+, NH +, Ca2+, Mg(H2O) 2+, Al(H2O) 3+ possible)

4 6 6

Red or red orange: Ca2+ (No Na , others may be present)

+

Purple: K+ (No Na and Ca , others may be present)

+
2
+

No color: possibly NH , Mg(H2O)6 , Al(H2O) (No Na , K+, Ca )

4
+ 2+
6
3+ + 2+

Green: Cu(OH2)62+

Color:__________________________________

CO32- or HCO3-
pinch of unknown with ~3 drops of 6M HNO3
Reasoning:
If you see bubbles, either CO or HCO is present (remember that carbonates interfere with flame
3
2-
3
-

test of solid Na and Ca salts)

Color:________________________________

2) Test for NH4+

Place a small portion of original sample in a test tube, then add a few drop of 6M NaOH
solution. Stir well then do sniff test (reliable and fast!); optional: do the litmus test (Red to blue).
Litmus Results:_____________________________

Sniff Results:______________________________

S2-/HS- Test
o Place original sample in a spot plate and add a few drops of 2M H2SO4, if a
rotten egg smell w/ bubbles, then S2- or HS- is present

_____________________________________

3) pH Test
pH:_______________

Meaning:
~1-2 HSO (No HCO , CO , OH )
4
- 3- 3- -

~3 (or lower) Al(H2O) (No HCO , CO , OH ) 6

3+
3
-
3
- -

~5 (or lower) NH , Mg(H2O) 4

+
6
2+

~7 Cl , NO , SO , K , Na , Ca (Note: neutral ions may be present at any pH)

-
3
-
4
2- + + 2+

~8.5 HCO (No HSO , Al(H2O) , OH )

3
-
4
-
6
3+ −

~12 CO3 (No HSO , Al(H2O) , NH )

-
4
-
6
3+
4
+

≥13 OH− (No HSO Al(H2O) , HCO , NH )4

-
6
3+
3
-
4
+

**If your sample has an insoluble compound, you just use the saturated supernatant liquid to test
pH. pH for insoluble compounds**
Ca(OH)2: ~ 12.6
CaSO4•2H2O: ~ 7.0
CaCO3: ~ 10.0
MgCO3: ~ 9.5
Mg(OH)2: ~ 10.5

Make solution
4. Make Solution
Dissolve 2/3 of sample with 10 mL deionized water. Stir well with a clean stirring rod for
20-30 seconds. Get a small amount of the supernatant and test its pH with pH paper (to
get the approximate pH), and indicator (to get the exact pH if needed).

• For 9A (which is a pure compound): 9A is either soluble or not, and cannot be

both.
Case 1: If the sample is soluble in water, then test the solution for cation and anion(s).
(Go to guide #1)

Case 2: If the sample is insoluble, then just test the insoluble compound. Discard the
supernatant (liquid portion). (Go to guide #2)

• For 9B (which may be a mixture),

Case 1: If the sample is FULLY soluble in water, then test solution for cation(s) and
anion(s).

Case 2: If it is insoluble or partially soluble, separate the solid from the supernatant
by using a centrifuge. Do not discard anything.
a. Test the supernatant for cation(s) and anion(s). Go to guide #1.
b. Test the insoluble portion. Go to guide #2.

Guide 1: Soluble Portion (Cations and Anions)

A. Cation Test
 Na+, K+, NH4+, Ca(OH2)62+,
Al(OH2)63+, Zn(OH2)62+,
Cu(OH2)62+, Ag(OH2)2+

Add 1 M NaCl dropwise (if no ppt forms after several drops, then no
Ag)

If ppt formed, add excess NaCl and remove AgCl ppt. by centrifuge.
Keep the supernatant(liquid)

To the supernatant, add excess 6M

NH3. Centrifuge.

Liquid: Na+, K+, NH4+, Ca(OH2)62+, PPT: Al(OH2)3(OH)3, Mg(OH)2

Al(OH2)63+, Zn(OH2)62+, Cu(OH2)62+,

Add 2-4 mL TAA+NaAc+ Add excess 2 M NaOH

heat (water bath)

White Ppt:
Soln: K+, Ca+
Ppt: CuS, ZnS Mg(OH)2

Add excess NaCO3 Add excess 2 M H2SO4 Soln:

Al(OH2)2(OH)4-
Ppt: CaCO3
Soln: Zn2+ ,odor Black ppt: CuS Add excess
Soln: K+ saturated NH4

Add NaCO3
Test for NH4 w/
litmus, burn off Ppt: Al(OH)3
NH4, test for K+ Ppt: ZnCO3
with cobaltinitrate

Ppt: K+ present
 B. Anion Test
• Cl-: Acidify with 3-6 drops 6M HNO3 then add AgNO3. If ppt. forms, then Cl is
present.
• SO42- and HSO4-: acidify with 3-6 drops 6M HNO3, then add Ba(NO3)2.
ppt =HSO4-/SO42- Go back to the pH result to determine what sulfate is present.
• NO3-: cover ferrous ammonia sulfate w/ solution. Add 3 drops 18M H2SO4. Red-brown
ppt = NO3 presence.
• OH-: Go back to the pH result.

Guide 2: Insolubles

A. Observe the color of the insoluble portion

• White: Ca(OH)2*, CaCO3*, CaSO4, Mg(OH)2*, Zn(OH)2*, ZnCO3, ZnO*, ZnS*,
AgCl, Ag2SO4 (soln in hot water?), MgCO3
• Black: CuO, CuS, Ag2O, Ag2S
• Dark Green: Ag2CO3
• Blue: CuCO3
*Soluble in 1M HNO3
B. Chemical test for insolubles (based on the color of the solid you have)
• Insoluble tests
o Dark brown, black, or dark green, CuCO3, CuO, CuS, Ag2CO3, Ag2O,Ag2S

CuCO3 Dissolved: Ag2 (add 1M NaCl to check)

CuO CuO (Blue Solution)

CuS Add 2 M HNO3

Bubbles and dissolved:
Ag2CO3 (hot water
Ag2CO3 (yellow soln, use NaCl to check)
bath T)
Ag2O CuCO3 (blue solution)
AgS
Nothing: Ag2S (+15 M HNO3- colorless
or yellow soln)

CuS (+15 M HNO3=blue solution)

 o White salts – Ca(OH)2, CaSO4*2H2O, CaCO3, Mg(OH)2, MgCO3
• Flame test – treat solid w/ 1M HCl, stir, and do a flame test.

• If flame is red-orange, then Ca2+ is present (If you are not certain repeat
flame test, but this time use 6M HCl). Then determine which is present
based on solubility in 1M HCl

Ca(OH)2 Dissolved- Ca(OH)2

CaSO4*2H2O Treat with

Nothing- CaSO4*2H2O
CaCO3 1 M HCl

Dissolves with bubbles- CaCO3

• If flame is colorless, do following chart:

Dissolves- Mg(OH)2, Zn(OH)2

Mg(OH)2

MgCO3 Dissolves with bubbles- MgCO3, ZnCO3

Zn(OH)2 Treat w/

2M H2SO4 Dissolves ZnS (rotten egg smell)

ZnCO3
AgSO4 (no smell)
ZnS

AgCl Nothing- AgCl

AgSO4