Introduction

The purpose of this practicum is to know the properties of the

elements and their ions in solution through observation. And Perform
cation analysis in a sample through group determination and specific
tests.
Qualitative analysis is an analysis that is carried out to find out what
elements are in a sample. Qualitative analysis for inorganic substances
consists of:
1. Anion Analysis
2. Cation Analysis
In cation analysis, the studied cations are as follows:
NH4 +, Na +, Ca2 +, Ba2 +, Mg2 +, Hg2 +, Pb2 +, Cu2 +, Sn2 +, Fe2 +,
Fe3 +, Co2 +, Mn2 +, Ni2 +, Al3 +, K +, Ag2 +, and so on.
The stages of the qualitative analysis carried out are as follows:
A. Preliminary Analysis.
In the sample, a "preliminary examination" is carried out, namely,
observing the physical properties, namely color, odor, crystal form, and a
water solubility test.

B. Test on.
To analyze a cation in the sample, a flame test can be performed.
Some metals have a specific flame color when heated in a bunsen flame
using Ni-Cr wire.

Table 3. Light Color on Metal Elements

Colour Metal
Carmine: Lithium Chompounds. Masked by Barium and
Red Sodium.
Scarlet or Crimsom: Strontium Compounds. Masked by
Barium.
Yellow-Red: Calsium Chompounds, Masked by Barium.
Sodium compounds, even in trace amount. A Yellow
Yellow flame is not indicative of sodium unless it persists and is
not intensified by addition of 1 % NaCl to the dry
compound.
White White-Green: Zink
Emerald: Copper compounds, other than halides. Thallium.
Green Blue-Green: Phosphates, when moistened with H2SO4 or
Br2O3.
Faint Green: Antimony and NH4 compounds.
Yellow-Green : Barium, Molybdenum
Azure: lead, selenium, bismuth, CuCl2 and other copper
Blue compounds moistened with hydrodoric acid.
Light-Blue : arcenic and come off it chompounds.
Grenish-Blue : CuBr2, antimony.
Pottasium chompounds other than borates, phosphates, and
Violet silicates. Masked by sodium or lithium.
Purple-red: Potassium, Rubidium, and / cessium , in the
precense of sodium when viewed through a blue glass.

Logam –logam Warna Nyala

Na Yellow
K Cobalt glass
Li Dark red
Ca Yellowish red
Sr Greenish yellow
Cu + Boraks Metal Green
 Pb, As, Sb, Bi Light Blue

C. Determination of the Cation Group

For systematic identification of cations, group separation must be
carried out. After that, a specific test is carried out for each cation in the
group to identify the presence in the sample. In this cation analysis there
are five groups:
 Group 1: Ag +, Pb2 + will precipitate as chlorine salt under strong
acid conditions.
 Group 2: Pb2 +, Hg2 +, CU2 +, Sn2 + will precipitate as sulfide or
hydroxide salts in a slightly acidic atmosphere.
 Group 3: Fe2 +, Fe3 +, Co2 +, Mn2 +, Ni2 +, Al3 + will precipitate as
sulfide or hydroxide salts in a slightly alkaline atmosphere.
 Group 4: Ca2 +, Ba2 + remain in solution after examination of cations
for group 1, 2, 3.
 Group 5: NH4 +, Mg2 +, K +, Na +.
Group 5 can be separated directly from groups 1 - 4, because H2S gas
has an unpleasant odor with harmful fibers, thiosetamide is used as a
substitute. The reaction of thiosetamide with water when heated will
also produce H2S, but it is a saturated solution.

E. Cation Analysis With Specific Reactions

a.Ag +
Ag + + Cl- → AgCl (s) ↓ white
Ag + + OH- → AgOH (s) ↓ black brown
AgOH + 2NH3 → (Ag(NH3)2)+ (l) dissolves in excess ammonia

b.Pb +
Pb2+ + CrO42- → PbCr4 (s) ↓ white
Pb2+ + SO2-→ PbSO4 ↓ white
Pb2+ + OH- → Pb(OH) (s) ↓ white. Does not dissolve in excess ammonia

c.Hg2+
Hg2+ + OH- → Hg2O(s) ↓ yellow
Hg2+ + 2I- → HgI2 ↓ red

d.Cu2 +
2Cu2+ + SO42- + 2NH3 + 2H2O → ↓Cu(OH)2.CuSO4 + 2NH4+
Cu2+ + 2OH- → Cu(OH)2 ↓ blue
Cu(OH)2 → CuO ↓ black + H2O
e.Sn2 +
Sn2+ + Hg2Cl2 → Hg2Cl2 ↓ white + Sn4+ + 2Cl-. If you add excess Sn2 +
Sn2+ + Hg2Cl2 → 2Hg ↓ gray + Sn4+ + 2Cl-

f.Fe2 +
Fe2+ + 2OH- → Fe (OH)2 ↓ white
4Fe(OH)2 + H2O + O2 → 4Fe (OH)3 ↓ brown red
Fe2+ + 3[Fe(CN)6]3- → ↓ Fe3+ + [Fe(CN)6]4-
4Fe3+ + 3[Fe(CN)6]4- → Fe4 [Fe(CN)6]3 ↓ blue turnbull

g.Fe3 +
Fe3+ + 3SCN- → Fe(SCN)3 ↓ dark red
3+ 3-
Fe + [Fe(CN)6] → Fe[Fe(CN)6] ↓brown
Adding H2O2 or a small amount of lead (II) chloride solution gives a
prussian blue precipitate.

h.Co2 +
Co2+ + 4SCN- → [Co(SCN)4]2- ↓ blue

i.Mn2 +
Mn2+ + 5NaBiO3 + 14H+ → 2MnO4+ + 5Bi3+ + 5Na+ + 7H2O
Produces the purple color of heat.

j. Ni2+

k. Al3+
Al3+ + 3 COO- + 2 H2O → Al(OH)2 CH3COOH ↓ + 2CH3COOH
Al3+ + 3OH- → Al(OH)3 ↓ white

l. Ba2+
Ba2+ + SO42 - → BaSO4 ↓ white
Ba2+ + CrO43- → BaCrO4 ↓ yellow

m. Ca2+
Ca2+ + SO42 - → CaSO4 ↓ white
Ca2+ + CrO42- → no sediment was formed
n. NH4+
NH4+ + OH- → NH3 naik + H2O
The smell arose, the red litmus paper turned blue

o. Mg2+
Mg2+ + NH3 + HPO43- → Mg(NH4) PO4 ↓ white crystalline

p. K+
3K+ + [CO(NO2)6]3- → K3 [CO(NO2)6] ↓ yellow

q. Na+
Na+ + Mg2+ + 3UO22+ + 9CH3COO- → NaMg(UO2)3 (CH3COO)9 ↓
yellow crystalline

Materials and Methods

Tools
 Reaction tube and rack 20,1
 Drop pipettes 8
 Measuring pipettes 5ml, 10ml 4,4
 100 ml measuring flask 1
 500ml chemical glass 1
 Watch glass 8
 Stirrer 1
 Spatula 1
 Aquadest bottle 4
 Bunsen, Tripod 1,1
 Rubber ball 4
 Masker 8
 Gloves 8
 Ni-Cr wire 1
Tool drawing (Attached)
Materials
Reagen
-   Tioasetamida                                       - Ba(NO3)2 0,1 M
-    (NH4)2CO3 in NH3 1 M                 - K4Fe(CN)6 0,5 M
-    NH4Cl 2 M                                          - K3(CN)6 0,5 M
-    HCl 6 M                                              - NaBi03 solid
-    NaOH 2 M                                          - KCNS solid
-    NaOH 6 M                                          - NaSO3 1 M solid
-    H2SO4 6 M                                          - KHSO4 solid
-    HNO3 1 M                                          - Na3(CO (NO2))6 solid
- Dimetilglioksim 1% in etanol - Morine solution

Snippet
-     AgNO3 0,1 M (Ag+) - Na2S 0,1 M (S-)
-     BaCl2 0,1 M (Ba+) - KSCN 0,1 M (K+/SCN-)
-     CuSO4 (Cu2+) - MnSO4 0,1 M (Mn2+/SO42-)
-     CaCl2 0,1 M (Ca2+) - SNCl2 0,1 M (Sn2+)
-     MnSO4 0,1 M (Mn2+) - (NH4)2 C2O4 (NH4+/C2O42-)
-     CoCl2 0,1 M (Co2+) - NiSO4 0,1 M (Ni2+)
 -     Al2(SO4)3 0,1 M (Al3+) - FeCl3 0,1 M (Fe2+)
-     Hg(NO3) 0,1 M (Hg2+) - KNO2 0,1 M (NO2-)
-     CH3COONa ( Na+/CH3COO-) - Kl 0,1 M (K+/I-)
-     CH3COOPb 0,1 M (Pb2+ /CH3COO-)          - CrCl3 0,1 M (Cr3+)
-     KBr 0,1 M (K+ / Br-)                                    - NaSO3 0,1 M (SO3-)
-     Mg(CH3COO)2 0,1 M (Mg2+ / CH3COO-)
Methods
- Preliminary Analysis
1.Physical observation
Make physical observations such as color, smell, and shape.
  Physical properties Color Smell Shape
Cation
Sample 1 White No smell Crystal
Sample 2 Blue No smell Crystal

2. Test solubility
Take 0.2 g of sample and add 2 ml of demineralized water. Observing
the solubility in cold water. When it doesn't dissolve, put the test tube into
a beaker containing boiling water. Observe and record the results of
observations, namely the color and pH of the solution.
If the sample does not dissolve in cold water or hot water, then
perform a solubility test with the following acids:
1 ml H2SO4 6 M
1 ml HCl 6 M
1 ml HNO3 6 M

Cation Cold water Hot water H2SO4 6 M HCl 6 M HNO3 6 M

1 √ - - - -
2 √ - - - -

3. Light Test
Put approximately 0.1g unknown sample on the watch glass and add
3 drops of 6M HCL. First, dip the wire into the HCL containing the
sample, then glow until the color is constant. Observing the characteristic
flame color, writing down the approximate elements that may be present.

- Cation Group Identification

Step 1: (Groups 1-4.5)
1 ml sample + 1 ml (NH4) 2CO3. When it settles, it means the cation
from groups 1-4. If it does not settle, it means group 5. Then do step 6.
Step 2: (Groups 1,2-4)
1 ml of sample solution + 3 drops of 6 M HCl. If there is a precipitate,
it is possible that Ag +, Hg +, Pb2 +. If it doesn't settle continue with step
3.

Step 3: (Groups 2,3-4)

1 ml of sample solution + drops of 6 M HCl and 1 ml of 1 M
Thiosetamide (pH 1). Putting the test tube for 5 minutes into a 250 ml
beaker filled with boiling water. The sulfur settling in the acid will be
perfect. If the precipitate is black, then the possibility of Pb2 +, Mg2 +,
Cu2 + cations, if the sediment is brown, it means Sn2 + cations. If it does
not settle, go to step 4. If there are oxidizing agents (Fe2 +, CrO42-), they
react with H2S to form colloidal sulfur (cloudy yellow).

Step 4: (Group 3,4)

1 ml of sample solution + 3 drops of 1 M NH4Cl and 1 ½ ml of NH3 6
M. Adding 1 ml of 1 M Thiosetamide Shake and bring to a boil for + 5
minutes. If there is a black precipitate, it means the possibility of Fe2 +,
Fe3 +, Co2 +, Ni2 + cations. If there is green sediment, it means Cr3 +. If
there is red sediment, it means Mn2 + sediment. If there is a white
precipitate it means the presence of Al3 +. If there are no deposits
continue with step 5.

Step 5: (Group 4)
Perform specific reactions to group 4 cations.

- Specific Reactions for Cation Analysis

Group 1:
1. Ag +
a. 1 ml of sample solution + 5 drops of 2M HCl 2M → ↓ white
The precipitate dissolves when 3/2 ml of NH3 6M is added and the
solution becomes clear.
b. 1 ml of sample + 2 drops of 1M NH3 → ↓ brown
Add ½ ml NH3 1M, the precipitate dissolves and the solution becomes
clear.
2.Pb2 +
a.1 ml sample + 4 drops of K2CrO4 0.1M → ↓ yellow
b.1 ml sample + 2 drops 1M NH3 → ↓ white , insoluble in excess NH3
Group 2:
1.Hg2 +
a.1 ml sample + ½ drop NH3 1M → ↓ cloudy yellow
b.1 ml sample + 1 ml KI 0.1 M → ↓ red cloudy

2. Cu2 +
1 ml sample + 2 drops 1 M NH3 → light blue
Adding excess ammonia (NH4OH 1M) occurs dark blue solution

3.Sn2 +
1 ml sample + 1 ml Hg (NO3)2 0.1M → ↓ white

Group 3:
1.Fe2 +
a.1 ml sample + 5 drops 2M NaOH → precipitate like brown gelatin
b.1 ml sample + 5 drops of K3Fe (CN) 6 → ↓ dark blue

2.Fe3 +
a.1 ml sample + 3 drops of 0.1 M KSCN → dark red
b.1 ml sample + 3 drops of K4Fe (CN) 6 0.5M → ↓ blue berlin

3.Co2 +
2 ml sample + 1 KSCN spatula → purplish blue.
Adding amyl alcohol ether turns blue.

4.Mn2 +
5 drops of sample + a tip of a sodium bismutate spatula + 5 drops of 6M
HNO3 → ↓ red violet

5. Ni2 +
1 ml sample + 2 drops of 1M NH3 + 1 ml dimethylglyoxime → ↓ red

6.Al3 +
a.1 ml sample + 3 drops CH 3COOH + a tip of a sodium acetate spatula +
1 ml of morine solution → green fluorescence
b.1 ml sample + 2 drops 2M NaOH → ↓ white.
Such as gelatin which can dissolve in excess NaOH

Group 4:
1.Ba2 +
a.1 ml sample + 5 drops 2M H2SO4 → ↓ white, insoluble in strong acids
b.1 ml sample + 5 drops K2CrO4 0.1M → ↓ light yellow

2.Ca2 +
a.1 ml sample + 4 drops (oxalate) → ↓ white
b.1 ml sample + 5 drops 2M H2SO4 → no sediment

Group 5:
1.Na +
If the reaction for the other cations in group 5 is negative and the flame
color is positive (within 1 minute), there is a Na atom.

2.K + / Na +
The tip of the spatula Na2 (Co(NO2)6) + ½ ml of water + 2 drops of 2M
CH3COOH → ↓ yellow

3.Mg2 +
1 ml sample + 4 drops of 1M NH 4Cl, 2M of NH4OH / NH3 and 1 ml of
0.1M of Na2HPO4 → ↓ white

4.NH4 +
1 spoon spatula snippet + 1 ml NaOH 6M heat, ammonia gas will be
released and can be identified by its smell.

Results and Discussion

Results
Reactor Observation Possible Cations
(NH4)2 CO3 Samples 1 and 2 settle
Sample 1 :
HCl 6M Samples 1 and 2 do not settle
Ba2+ and Ca2+
and form a solution
Sample 2 :
HCl 6M and Sample 1 doesn’t settle and a Hg2+, Cu2+, and Sn2+
tiosetamida solution is formed, sample 2
doesn’t settle
NH4Cl 1M Sample 1 didn’t settle and a
and NH3 solution was formed
 Based on the experiments that have been carried out, sample 1 has a
white color, is crystalline, odorless and dissolves in cold water. whereas
sample 2 is blue, crystalline, odorless, and dissolves in cold water.
After that proceed with the identification of the cation group. The
cation group consists of 5 groups and we have to do a specific reaction to
find out the cation from the sample given. For cations from group 5 a
flame test should be performed. Because the snippets we get do not come
from group 5, a flame test is not carried out. After taking observational
steps, it was found that sample 1 came from group 4 and sample 2 from
group 2.

Discussion
From the experiments and observations made, we can identify the
properties of the elements and their ions by observing whether there is
any sediment in the sample. It was found that:
1. Sample 1 is group 4 Ba2 + cations
2. Sample 2 is group 2 Cu2 + cation

Attachment

Reaction tube and rack Drop pipettes Measuring pipettes

Watch glass
Measuring flask Chemical glass
 Stirrer Spatula Aquadest bottle

Rubber ball Bunsen Tripod

Ni-Cr wire Masker Gloves