Group # 10
ESPINOSA, Elise Angela H.
MANUEL, Immary Alleivin R.
SALT SAMPLE:
Cd(CH3COO)2
LIQUID SAMPLE INCLUDES:
Fe2+ (possibly oxidized to Fe3+)
and K+
Soluble in Water
Dissolve a pinch of sample in water
Add a few drops of Sodium Carbonate
**
Precipitation? Proceed to
Step 2.
No Precipitation? Proceed
to Anion Preliminary
Tests.
Insoluble in Water
Add 3mL of Sodium Carbonate to a
small amount of test sample
Heat for 5 mins. Centrifuge and
Decant. Use decantate for Anion Test.
Add little
Sulfuric Acid
to a small
amount of
unknown
sample
Note all
observations
like gas and
product
formation,
change in
color, etc.
If no change
occurs, warm
the test tube.
ANIONS
VISIBLE RESULT
REACTION EQUATION
Carbonate
Gas formation
CO32- + 2H + CO2 + H20
Oxalate
Gas formation
C2O42- + 2H+ H2C2O4
Sulfide
Rotten egg odor
Chloride
Fumes in moist air
Cl- + H2SO4 HCl + HSO4-
Bromide
Reddish brown color
Br- + H2SO4 HBr + HSO4-
Iodide
Violet color; fumes in moist air
I- + H2SO4 I2 + H2S H2O
Chromate
Yellow to Orange change in color
2CrO42- + 2 H+ Cr2O72- + H2O
Nitrite
Evolution of brown fumes
NO2- + 4H+ 4NO + 2H2O + O2
S2- + 2H+ H2S
ANIONS
VISIBLE RESULT
REACTION EQUATION
Acetate
Gas formation; vinegar-like
smell
OAc- + H+ HOAc
Nitrite
Evolution of brown fumes;
strong odor
4NO3 + 4H2SO4 2SO42- + 4H2O
+ 4NO2
Add Silver
Nitrate.
Precipitation?
Centrifuge and
Decant (C&D).
Wash the
residue with
water. Add
Nitric Acid.
C&D.
To the
decantate,
add
Ammonia
and Silver
Nitrate.
Yellow ppt =
phosphate
Red ppt =
chromate
Add Ammonia
until basic to
unknown
sample. Ppt? C
& D. Discard
the residue.
Add Barium
Chloride and
Calcium
Chloride. No
precipitate?
Sulfate,
chromate,
phosphate
and oxalate
are absent.
Yellow
precipitate?
Chromate
might be
present. Add
HCl until
acidic. If
everything
dissolved,
sulfate is
absent.
Carbonate
Disregard if no effervescence occured
in Sulfuric Acid Test
Chromate &
Permanganate
Disregard if unknown sample is
colorless
CNS--
Add Fe(NO3)3.
Formation of blood-red
solution confirms thiocyanate.
Fe3+ + CNS- FeCNS2+
FeCNS2+ is a complex ion and is responsible for
the formation of the blood red solution
I-Acidify with HNO3. Add Fe(NO3)3 and CCl4. Shake.
Purple layer confirms iodide. If no iodide is
present, proceed to bromide confirmatory
test.
If iodide is present, remove CCl4 layer and add new CCl4
and Fe(NO3)3. Remove violet CCl4 layer. Repeat until no
iodide is present. Proceed to bromide confirmatory test.
Br-To the solution from Iodide test, add
equal amount of HNO3. Heat then cool in
cold water.
Add CCl4. Shake thoroughly.
Yellowish/Reddish layer confirms bromide.
Discard bromide layer. Proceed to Choride
test.
Cl-Acidify test solution from bromide test
with HNO3.
Add water and AgNO3.
White precipitate confirms
chloride.
I , Br & Cl
*Iodide, Bromide and Chloride are ionic while CCl4 is
non-polar.
*Purple immiscible layer is formed for Iodide.
*Yellowish brown immiscible layer is formed for
Bromide (due to oxidation: Br- Br2)
*White precipitate is produced for Chloride because
AgCl is formed.
S2Place a small amount of unknown
sample in a small beaker. Add HCl.
Moisten a small piece of filter paper with lead
acetate. Place it on the convex side of a watch
glass. Cover the beaker with the watch glass.
Heat gently. If filter paper turns
black/silvery, sulfide is present.
S2-
(a) H+ + S2- H2S
(b) Pb2+ + S2- PbS(s)
H2S reacts with lead acetate forming
PbS which is responsible for the
black/silver color.
CO32Prepare a glass medicine dropper with a
drop of barium hydroxide suspended at
the tip.
Cover a test tube with unknown sample with
the medicine droper. Warm but not boil.
Observe the droplet. If it becomes
cloudy/white, carbonate is confirmed.
CO32-
CO2(g) + Ba2+(aq) BaCO3(s) + H2O
*Carbonates are soluble in acids,
producing Carbonic Acid
*Addition of barium hydroxide reacts
with carbonic acid, forming BaCO3, which
is the cloudy/white precipitate
SO42-
Add HCl until acidic then add
excess HCl. Add BaCl2.
White precipitate confirms
sulfate.
Sulfates dont easily react but it reacts with Ba2+.
Addition of BaCl2 reacts with sulfate forming Barium Sulfate
SO42-(aq) + Ba2+(aq) BaSO4(s)
CrO42Add 1M HNO3 until acidic. Add 3M HNO3
until a layer forms.
Add fresh hydrogen peroxide. Shake once
quickly.
Formation of blue color
confirms presence of chromate.
CrO42-
(a) 2CrO42- + 2H+ Cr2O72- + H2O
(b) Cr2O72-(aq) + 4H2O2(aq) + 2H+(aq)
2CrO5(aq) + H2O
*Chromates react with acid and is converted to
dichromate
*Dichromate reacts with H2O2 which causes the
fading of color
PO43-
Add 16M HNO3 and ammonium
molybdate. Warm in a water
bath.
Yellow precipitate
confirms phosphate.
PO43-
H3PO4(aq) + 12 MoO42-(aq) + 3 NH4+(aq) + 22H+(aq)
(NH4)3PO4 12 MoO3(s) + 12 H2O
*Phosphates are generally stable although
there are exceptions: FePO4, CrPO4, BiPO4,
Ca3(PO4)2 and AgPO4
*Yellow color is caused by the formation of
ammonium phosphomolybdate
C2O42Add 6M HOAc and CaCl2. Precipitation?
C&D.
Wash precipitate with water. Discard washing.
Add water, KMnO4 and H2SO4.
If permanganate color fades in
30 seconds, oxalate is present.
C2O42-
5C2O42-(aq) + 2MnO4-(aq) + 8H+(aq) 10CO2(g) +
2Mn2+(aq) + 4H2O
*Oxalates are soluble in acidic solutions
*Addition of permanganate causes the
conversion of oxalate to CO2 gas
* Fading of permanganate color is caused by
the CO2 gas
CH3COO-Add 1:1 sulfuric acid to water solutionn.
Vinegar-like odor? Acetate is present
No vinegar odor? Add 2 drops ethyl alcohol.
Warm gently. Sniff cautiously.
Presence of sweet alcohol
smell confirms acetate.
CH3COO--
CH3COO- + H2SO4 CH3COOH + HSO4*Vinegar-like smell is due to the conversion
of acetate to acetic acid upon the addition
of sulfuric acid.
NO3--
Add concentrated sulfuric acid and
a grain of ferrous sulfate. Wait for
a few minutes.
A brown ring formation
confirms nitrate.
NO3--
(a) 3Fe2+(aq) + NO3-(aq) + 4H+(aq) 3Fe3+(aq) + NO(aq) + 2H2O(l)
(b) Fe2+(aq) + NO(aq) Fe(NO)2+(aq)
*Nitrate oxidizes Fe2+ to Fe3+
*Nitrogen (IV) oxide gas is produced which is
responsible for the brown ring formation
S2O32-
Add 3M HCl.
A cream/whitish precipitated
confirms thiosulfate.
S2O32-
S2O32-(aq) + 2H+(aq) SO2(g) + S(s) + H2O
*Thiosulfate decomposes into sulfite and
elemental sulfur
*Elemental sulfur, S , is the white precipitate
formed
NO2--
Add 6M HOAc until acidic. Add
K3Fe(CN)6. Let it stand for 1
minute.
Add 1 drop FeCl3. Deep red
precipitate confirms nitrite.
NO2--
(a) HNO2(aq) + Fe2+(aq) + H+(aq) Fe3+(aq)
+ NO(aq) + H2O
(b) NO(aq) + Fe2+(aq) Fe(NO)2+(aq)
*Nitrites are converted to nitrous acid whenever an
acid reacts with nitrites
*Deep-red solution is caused by complex ion
Fe(NO)2+
MnO4--
Add water and sodium oxalate
and sulfuric acid/
Color disappearance within
30 seconds confirms
presence of permanganate.
MnO4
5C2O42-(aq) + 2MnO4-(aq) + 8H+(aq) 10CO2(g) +
2Mn2+(aq) + 4H2O
*Similar to oxalate test
*Formation of CO2 gas occurs which cause
the permanganate color to fade
Qualitative Analysis = used in identifying
the presence of a substance in an unknown
solution
Different concepts and techniques have to
be applied
Conclusions are made after every procedure
performed
Follow the procedure very carefully and accurately
Observe ALL possible reactions
Observe CLEANLINESS at all times so as to prevent
contamination
Work efficiently and precisely in order to minimize
human error.
-FIN-
