I.

Title Of The Experiment : Analysis of cation and anion

II. Experiment Date : Monday, March 13, 2023
III. Experiment Time : 09.30 – 12.00
IV. Experiment Purpose : 1. Determine the cation in the analyte
2. Determine the anion in the analyte
V. Literature Review
1. Apparatus used in the Chemical Analysis and their functions
It is preferable to use small amounts of chemicals in the chemical analysis
as this is economical in the consumption of these chemicals and the
detection takes a shorter time. Apparatus includes the following :
a) Test Tubes and Centrifuge Tubes: The use of circular-end pipes for the
testing and shroud type of Pyrex (heat resistant) in the case of heating
b) Droppers used to transferring solutions and reagents from bottles, there
are different types of droppers.
c) Reagents Bottles.
d) Centrifuge To separate the precipitant from the solution. The solution
could be placed either in a test tube or a centrifuge tube in one of the
spaces in the rotor and in the opposite space, place a balancing tube
i.e., a tube of the same size filled with an equal volume of water to that
of your solution.
The Benefit of Using Centrifuge
- Speed and accuracy.
- To concentrate on the precipitate to a small volumes can be quantified.
- Quickly and efficiently wash the precipitate
e) Wash Bottles, i.e., filed with distilled water: it is used by pressing it
with hands.
2. Practical Rules
a) Heating Solutions
Do not heat the centrifuge tube on the fire directly so that it could
affect the content of the tube and cause serious damage, especially in
the case of acids and bases. It is advisable to heal it on a water bath.
Do not heat the ordinary glass on a Bunsen burner or other heat source
 because it breaks when exposed to heat and uses glass made of Pyrex
or porcelain.
b) Dissolving the Precipitate
The reagent is added to the precipitate and heated in a water bath until
the precipitate dissolves completely or partially In the latter case, the
precipitate is separated from the solution by the insoluble force
c) Cleaning Glassware
The laboratory glassware is cleaned by washing them firstly with
detergent and tap water followed, then rinsed with distilled or
deionized water, then dried with a hydrochloric acid solution (2%) or
dichromate solution (10%) and 10 ml concentrated sulphuric acid. To
remove hard precipitates from dirty glassware, the nitric acid solution
can be used (Roy, 2021)1.
3. Type of Chemical Analysis
a) Qualitative Analysis
It is defined as a set of tests or chemical processes aimed to identify
the material whether unknown material is a the substance or mixture in
a solid state or in a solution without paying attention to the weights of
these components or the elements involved in the structure or the
proportions of their existence. Therefore, the descriptive analysis is
never affected by the loss of the sample for a fraction of its quantity as
long as the purpose of this analysis is to determine the components of
the relative presence or weights in the sample.
b) Quantitative Analysis
It is used to determine the weights of the components or elements
involved in the composition of the mixture or the chemical compound
and its proportions. Therefore, the presence of impurities in the
material affects the determination of these weights and the choice of
analysis method that requires knowledge of the elements that made up
the substance under investigation.
There is no real difference between micro qualitative analysis and
semi-micro qualitative analysis, which is the result of the difference in
 the quantities used in the two cases. The difference is confined to the
quantities and small volumes of the sediments and solutions that are
used, as well as the use of the type of special tools for each analysis.
There is no advantage in the sensitivity of the semi-micro qualitative
analysis However, there are a number of advantages in another aspect,
for example, saving time and chemicals. Filtration, sediment washing,
and vaporization processes can take about an hour. These processes
can be performed in a few minutes if the semi- micro-method is
followed, thus allowing the student to analyse more samples on time
and gain broader training in analytical methods.
4. Glossary in Qualitative Analysis
a) Centrifuge: It is a device used to accelerate the stability of the
sediment, making use of centrifugal force.
b) Suspension: It is the separation of liquid from stable sediment.
c) Filtration: It is the separation of a precipitate from a fluid through a
medium. A liquid that passes through the filter called filtrate or filtered
liquid, while the residue left on the filter paper is called filtered solid
(separation processes are often done in semi-micro-analysis by
centrifuge and circulation).
d) Sedimentation: It is the formation of an insoluble solid that forms
when reagent reacts with a solution. The insoluble solid is called a
precipitate.
e) Reagent: It a substance used to make a chemical change in the material
under test, for example, hydrochloric acid is a reagent added to the
solution of silver nitrate because it is a precipitate of silver chloride.
f) Turbidity: It is the occurrence of something like clouds as a result of
small particles stuck in a solvent.
g) Washing: It is the cleaning of precipitate (usually with water) to
remove the suspension of the solution from which it precipitates
(Muntean, 2022)2.
5. Rules of solubility of inorganic compounds
 As the solubility of matter in water is important to be taken into
consideration in the analysis, the student must be familiar with the
following rules of solubility :
a) All salts of hydrochloric acid (chlorides) and hydro-bromic (bromides)
are soluble in water as well as hydro-iodic acid (iodides) other than
salts associated with Ag+, Hg22+, Pb2+ [lead (II) chloride and lead (11)
bromide are mild soluble in cold water and dissolved in hot water]
b) All nitrate NO3-, nitrite NO2-, and acetic salts are soluble in water.
c) All sulphate salts are dissolved in water except barium sulphate,
strontium sulphate and lead (II) sulphate (BaSO4, SrSO4, and PbSO4),
which are mild soluble in water.
d) All sodium, potassium and ammonium salts are soluble in water except
for some complex salts.
e) All oxides and hydroxides are poorly soluble in water except oxides
and hydroxides of alkali and alkaline earth metals, ammonium
hydroxide and barium hydroxide, strontium hydroxide and calcium
hydroxide, which are mild soluble in water.
f) All silicates are insoluble in water except alkaline metal silicate.
g) All cyanides are insoluble in water except alkaline cyanides and
mercury (II) cyanide.
h) All sulphide salts (salts derived from H2S) are poorly soluble in water
except alkali metal sulphide, ammonium sulphide and alkaline earth
metal sulphide.
i) All carbonates, phosphates, urea, oxalates, chromates, resins, iron, and
cyanides are either insoluble or low-soluble except for the alkali and
ammonium metals but they readily dissolve in the achieved acids. The
carbonates and acid phosphates such as Ca(HCO3)2, Ca(H2PO4)2 and
others are dissolved in water.
6. Group separation and identification of the cations
A small number of carbonates can be detected in the presence of a few
other cations. For example, adding hydrochloric acid to a solution
containing all cations, only the lead, silver and mercury are precipitated,
because all other chlorides are soluble (see solubility rules). Then lead,
silver and mercurous (Mercury I) are a group of ions that can be
precipitated in the solution by adding the group reagent (HCI). After
separating this group of ions, another group can be precipitated by adding
the reagent of this group.
There are 28 radical cations that will be separated during the detection and
investigation of the identity of the unknown cation and are divided into
five major groups depending on the variation in some of their chemical
properties. There are four groups by special regrant in certain
circumstances, while the fifth group is in the form of a solution, which led
to the name of the soluble group.
There are principles used to explain the sequential steps and the conditions
that enhance the group precipitate are shown in Flow chart 2.1 since all
cations are present in the solution together as a mixture.
a) All cations in solution are transformed by reacting with hydrochloric
acid into chlorides in an acidic medium. Cations that do not dissolve
their chlorides in water are the first group chlorides consisting of silver
Ag+, lead Pb2+ and mercurous Hg22+, unlike chlorides of other
dissolved groups in water.
b) The cations of the second group containing Bi3+, Cd2+, Cu2+, Hg2+,
Pb2+, Sn4+, Sn2+, Sb3+, As3+) are precipitated from their dissolved
chloride solution as sulphides using H2S directly or indirectly (as a
thioacetamide analysis that gives H2S. Hydrochloric acid is used to
control the concentration of H3O+ (0.2-0.3 M). It is important to know
the concentration of sulphide ion that comes from HS which is enough
to precipitate the second group cations leaving other cations in another
group (3-5) that are soluble in solution
c) The third group contains (Co2+, Cr3+, Fe2+, Fe3+, Al3+, Zn2+, Mn2+,
Ni2+) which are separated after precipitation as a mixture of insoluble
hydroxides and sulphides using two precipitators: ammonia, H2S or
thioacetamide in a moderate basic solution consisting of ammonium
hydroxide and ammonium chloride, where ions (Zn2+, Co2+, Fe2+, Ni2+,
 Mn2+) are precipitated as sulphides while ions (Al3+, Fe3+, Cr3+) are
precipitated in the form of hydroxides.
d) The fourth group consists of ions (Calcium Ca2+, Strontium Sr2+, and
Barium Ba2+) These ions are within a single group in the periodic
table. Therefore, they are similar in their chemical reactions and their
valence electrons Their components are reductive agents, their ions
appear only slightly inclined to form complexities and they do not
degrade in water. Among the ions (Ca2+, Sr2+, Ba2+). It is difficult to
make a good separation between them. The ions of this group are
separated from the fifth group in one of the two ways:
i. The phosphate ion PO43- is added as a precipitating agent in a
high concentration of ammonia solution as a consequence of
that (Ca2+, Sr2+, Ba2+), ions are precipitated in a general
phosphate form (M3(PO)4)2) while magnesium is precipitated
as Ammonium magnesium phosphate NH4MgPO4.6H2O.
ii. The carbonate ion CO32- is added as a precipitating agent to the
group ions and then the magnesium ion will be the fifth group
(v) ammonium NH4+, sodium Na+, potassium K+, magnesium
Mg2+. The cations of this group are not precipitated in any
reagent, but they can be precipitated by some specific reagent
(Alhasan dkk., 2021)3.
7. Identification of the anions
The method of introducing anions is not as systematic as in the
introduction of cations. One way of classifying anions is the separation of
anions based on the solubility of silver salts, calcium salts, barium and
zinc. In addition, there is a way of classifying anions according to Bunsen,
Gilreath and Vogel. Bunsen classified anions according to their solubility
of silver and barium salts, color, solubility of alkali salts, and volatility.
Gilreath classifies anions based on the solubility of their Ca, Ba, Cd salts
and silver salts. While Vogel classifies anions based on the process used,
namely the examination of anions based on their reactions in solution.
 Examination of anions that evaporate when treated with dilute HCl
or dilute H2SO4, and anions that form gas when treated with concentrated
H2SO4. Likewise, the examination of anions based on their reactions in
solution is divided into two, namely the anions examined by precipitation
reactions and the anions examined by their redox reactions. Anion
examination includes the continuation of preliminary analysis, anion
analysis of the original substance and anion analysis using extra soda
solution. The results of the preliminary analysis (solubility data) and
knowledge of the cations present can provide clues as to which anions may
or may not be present in the sample solution (Kunsah dkk., 2019)4.

VI. Tools and Materials

• Tools
1. Test tube 5 mL 5
2. Plastic dropper pipette 1 mL 5
3. Centrifuge tube 1
4. Filter paper enough
5. Tripod + gauze 1
6. Beaker 250 mL 1
7. Tube clamp 1
8. Test tube rack 1
9. Stirrer 1
10. Spirit burner 1
11. Centrifuge tool 1
• Material
ANALYSIS OF CATIONS
1. Sample (solution)
2. HCl 6M
3. Saturated HCl
4. CH3COOH 6M 2 drops
5. K2CrO4 1 drops
6. Ammonium hydroxide 6M
7. Saturated HNO3
8. Aquades
ANALYSIS OF ANIONS
1. Sample (solution)
2. Na2CO3 saturated
3. Concentrated H2SO4
4. Saturated FeSO4
5. AgNO3
6. BaCl2
7. NH4OH 6M
VII. Sceme / Work Flow
1) Analysis of group 1 cations

Sample Solution

1. Added some drops of HCl 6 M

2. Added 2 drops of aqueous HCl
3. Centrifuged and clean off the
precipitate

Precipitates Group II, III, IV, V

Filtrate
4. Cleaned the precipitates
5. Heated on boiling water bath
6. Centrifuged

Pb2+ Filtrates

7. Added with 2 drops of 6M CH3COOH

8. Added with 1 drop of K2CrO4

Yellow colored Precipitates

precipitates PbCrO4
7. Dissolved in 0,5
mL NH4OH 6M
8. Heated
9. Stirred
10. Centrifuged

Filtrate Black precipitates

Hg(NH2)Cl + Hg

11. Added with HCl or Aqueous HNO3

White
precipitates AgCl
Reactions :

1. Pb2+ + 2Cl- → PbCl2 ↓

2. Ag+ + Cl- → AgCl ↓

3. Hg2+ + 2Cl- → HgCl2 ↓

4. Pb2+ + CH3COO- → Pb(CH3COO)2

5. Pb2+ + CrO42- → PbCrO4 ↓ (yellow precipitate)

6. Hg2Cl2 + 2NH3 → Hg ↓ + Hg(NH3)Cl ↓ + NH4+ + Cl- (black precipitate)

7. AgCl ↓ + 2NH3 → [Ag(NH3)2]+ + Cl-

8. [Ag(NH3)2]+ + Cl- + HNO3 → AgCl ↓ + NH4NO3

9. [Ag(NH3)2]+ Cl- AgCl ↓ + NH4+ (White precipitate)

 2. Analysis Anions
a) Prepare a preparatory solution
Sample

1. Heated with saturated

Na2CO3
2. Filtered its precipitate

Precipitate (Not used) Preparation solution

SO42- Cl- I- SO32- PO43- CH3COO-

NO3- Br S2- S2O32- CO32-

-

b) Proof of sulfate ions (SO42-)

Prepare solution
1. Added 6 M HCl solution until it
become acidic
2. Brought to a boil
3. Added BaCl2 solution
White precipitate BaSO4

Reaction :
1. SO42- + Ba2+ → BaSO4
2. BaSO4 + 4C + Na2CO3 → Na2S + BaCO3 + 4CO ↓
3. Na2S → 2Na + S-
4. 2S- + 4Ag + O2 + 2H2O → 2Ag2S↓ + 4OH-

c) Proof of nitrate ion (NO3-)

Preparation solution

1. Added concentrate H2SO4 solution

2. Added saturated FeSO4 solution slowly
through the tube wall
Brown ring
Reactions :
1. 4NO3- + 2H2SO4 → 4NO2 ↑ + O2 ↑ + 2SO2- + 2H2O
2. 2NO3- + 4H2SO4 + 6Fe2+ → 6Fe3+ + 2NO ↑ + 4SO42- + 4H2O
3. Fe2+ + NO ↑ → [Fe(NO)]2+
 d) Proof chloride ion (Cl-)
Preparation solution

1. Added AgNO3 solution

White precipitate

2. Added ammonia solution

Dissolved white solution

Reactions :
1. Cl- + Ag+ → AgCl ↓ (White)
2. AgCl↓ + 2NH3 → [Ag(NH3)2]+ + Cl-
3. [Ag(NH3)2]+ + Cl- + 2H+ → AgCl ↓ + 2NH4+
 VIII. Observation Result

No. Result Experiment Assumption/React

Experiment Procedure Conclusion
Trial Before After ion
1. Cation Analysis Sample X (BE) and Y (CD) Group I - Sample X (BE) = - Sample X solution + 1. Pb2+ + 2Cl- → Sample X in this
PbCl2 ↓
Sample white/cloudy 4 drops HCl 6M + 2 experiments,
1. Added a few drops of 0.6 M HCl
2. Ag+ + Cl- →
2. Added 1-2 drops of dilute HCl solution drops aqueous HCl = AgCl ↓ sample solution
2+ -
- Sample Y (CD) white/cloudy solution 3. Hg2 + 2Cl → doesn’t contain
Precipitate Filtrate HgCl2 ↓
PbCl2, AgCl, Hg2Cl2 Group II/II/IV/V = colourless - Centrifuged = White 4. Pb2+ + Pb and Hg, but
3. Washed solution precipitate and CH3COOH- → contain Ag+. This
4. Heated in a water bath 1 minute Pb(CH3COOH)2
5. Centrifuged
- 6M HCl = colourless filtrate 5. Pb2+ + CrO42- → characterized by
colourless (Group II, III, IV, PbCrO4 ↓ the presence of a
Filtrate Pb2+ Precipitate
(yellow
6. Added 2 drops of 8. Dissolved in 0.5mL NH4OH 6 M solution and V) white precipitates
CH3COOH solution
precipitate)
9. Heated
7. Added 1 drop of chromat - Dilute / aquoeus - White precipitate 6. Hg2Cl2 + 2NH3
10. Stirred
potasium solution → Hg ↓ +
11. Centrifuged HCl = colourless washed, heated, Hg(NH3)Cl Sample Y in this
Yellow precipitate
solution centrifuged = white (black experiments,
PbCrO4 precipitate) +
Filtrate Black Precipitate - 6M CH3COOH = precipitated and NH4+ + Cl- sample solution
t 12. Added HCl or dilute Hg(NH2)Cl + Hg
colourless colourless filtrate 7. AgCl ↓ + 2NH3 doesn’t contain
HNO3
→ [Ag(NH3)2]+
White precipitate
solution - Filtrate + CH3COOH +Cl- Hg and Ag, but
AgCl - K2CrO4 = yellow + K2CrO4 = yellow 8. [Ag(NH3)2]+ + contain Pb2+. This
Cl + HNO3 →
solution AgCl ↓ + characterized by
- 6M NH4OH = filtrate (not contain NH4NO3 the presence of a
9. [Ag(NH3)2]+ +
colourless Pb2+) yellow
Cl- ⇌ AgCl ↓ +
solution - Precipitate + 0,5 mL NH4+ (white precipitates
- Aquades = NH4OH + heated + precipitate)
(Svehla, 1979)
colourless centrifuged = there is
solution a colourless filtrate
and grey precipitate
(not contain Hg2+)
- Filtrate + 4 drops of
dilute/aqueous HCl =
white/cloudy filtrate
but after few minutes
there is have white
precipitates (presence
Ag+)

- Sample Y solution +
4 drops HCl 6M + 2
drops aqueous HCl =
white/cloudy solution
- Centrifuged = White
precipitate and
colourless filtrate
(Group II, III, IV,
and V)
- White precipitate
washed, heated,
centrifuged = white
precipitated and
colourless filtrate
- Filtrate + 2 drops of
CH3COOH + 1 drops
of K2CrO4 = yellow
precipitate ang
yellow filtrate
(contain Pb2+)
- Precipitate X + 2,5
mL NH4OH + heated
+ centrifuged = there
is a colourless filtrate
 and grey precipitate
(not contain Hg2+)
- Filtrate + 4 drops of
dilute/aqueous HCl =
colourless filtrate
(not contain Ag+)
2 Anion Analysis Sample X (BE) and Y (CD) - Sample X = Preparation Solution In this experiment
Making a preparation solution white/cloudy X for sample X

Sample
solution - Sample X + Na2CO3 contain SO42- as

1. Heated with saturated - Sample Y = = brown precipitates seen presence of a

Na2CO3
2. Filtered its precipitate colourless and cloudy brown white precipitate
solution filtrate and contain NO3-
Precipitate (Not used) Preparation solution - Na2CO3 = - After Heated sample as seen presence
3. Devided into 11 test tube
colourless = brown precipitates of a brown ring.
SO42- Cl- I- SO32- PO43- CH3COO- solution and colourless filtrate While for sample
NO3- Br S2- S2O32- CO32- Preparation Solution Y just contain
-

Y NO3- as seen by
- Sample Y + Na2CO3 the presence of a
= white precipitates brown ring.
 and cloudy white
filtrate
- After Heated sample
= white precipitates
and colourless filtrate

Proof of Sulfate ion (SO42-) - Preparation - Filtrate X + 6M HCl - SO42- + Ba2+ →

BaSO4
Prepare solution solution X = = colourless filtrate
- BaSO4 + 4C +
brown (there is a bubbles Na2CO3 → Na2S +
1. Added 6 M HCl solution until it
BaCO3 + 4CO ↓
become acidic precipitates and like boiling)
- Na2S → 2Na + S-
2. Brought to a boil cloudy brown - Filtrate after boiling = - 2S- + 4Ag + O2 +
3. Added BaCl2 solution 2H2O → 2Ag2S↓ +
filtrate cloudy filtrate
White precipitate BaSO4 4OH-
- After Heated - Filtrate X + BaCl2 = (Svehla, 1979)
sample = brown cloudy filtrate and
precipitates and white precipitate
colourless filtrate (presence of SO42-)
- Preparation
solution Y = - Filtrate Y + 6M HCl
white = colourless filtrate
 precipitates and (there is a bubbles
cloudy white like boiling)
filtrate - Filtrate after boiling =
- After Heated coourless filtrate
sample = white - Filtrate Y + BaCl2 =
precipitates and colourless filtrate and
colourless filtrate not have precipitate
- 6M HCl = (not presence of SO42-
colourless )
solution
- BaCl2 =
colourless
solution
Proof of Nitrate ion (NO3-) - Preparation - Filtrate X + 8 drops - 2NO3- + 4H2SO4 +
6Fe2+ → 6Fe2+ +
solution X = of H2SO4 =
Preparation solution 2NO ↑ 4SO42-
brown colourless filtrate 4H2O
1. Added concentrate H2SO4 solution - Fe2+ + NO ↑ →
2. Added saturated FeSO4 solution slowly precipitates and (there is a bubbles
[Fe(NO)]2+
through the tube wall cloudy brown like boiling) (Svehla, 1979)
Brown ring filtrate - Filtrate X + 5 drops
FeSO4 = colourless
- After Heated filtrate and brown
sample = brown ring (brown ring
precipitates and presence of NO3-)
colourless filtrate
- Preparation - Filtrate Y + 14 drops
solution Y = of H2SO4 =
white colourless filtrate
precipitates and (there is a bubbles
cloudy white like boiling)
filtrate Filtrate Y + 9 drops
- After Heated FeSO4 = colourless
sample = white filtrate and brown ring
precipitates and (brown ring presence
colourless filtrate of NO3-).
- H2SO4 =
colourless
solution
- FeSO4 = Yellow
solution
Proof of Chloride ion (Cl-) - Preparation - Filtrate X + AgNO3 = - Cl- + Ag+ → AgCl
↓ (White)
solution X = colourless filtrate and
- AgCl↓ + 2NH3 →
brown white precipitate [Ag(NH3)2]+ + Cl-
Preparation solution
precipitates and - Filtrate X + NH OH = (Svehla, 1979)
4
1. Added AgNO3 solution cloudy brown cloudy filtrate and
White precipitate filtrate white precipitate
- After Heated (presence precipitate
2. Added ammonia solution
sample = brown means no Cl-)
Dissolved white solution precipitates and
colourless filtrate - Filtrate Y + AgNO3 =
- Preparation colourless filtrate and
solution Y = white precipitate
white Filtrate Y + NH4OH =
precipitates and cloudy filtrate and
cloudy white white precipitate
filtrate (presence precipitate
- After Heated means no Cl-)
sample = white
precipitates and
colourless filtrate
- AgNO3 =
colourless
solution
- NH4OH =
colourless
solution
IX. Analysis and Discussion
Cations are ions that have a positive charge because they lose electrons,
while anions are ions that have a negative charge because they gain electrons.
The purpose of this practicum is to find out the cation and anion groups of a
given analyte. The analysis used in this experiment is qualitative analysis. The
basic principles of cation and anion analysis are based on precipitation,
neutralization, complex formation, and reduction reactions.
a. Cation Analysis
In the first experiment, cation analysis was carried out on 2 solution
samples which are group I, namely CD sample solution and BE sample
solution. The cations of group I include Pb2+, Hg22+, and Ag+. The first step is
to take a few milli sample solution into a test tube, then add a few drops of
6M HCl and 2 drops of diluted HCl. The solution is homogenized so that it
changes color to turbid white and a white precipitate is formed. The purpose
of adding diluted HCl is to ensure that all group I cations precipitate. Next,
the solution is centrifuge for ±2 minutes with the aim of separating the
precipitate from the filtrate. Then the precipitate is separated from the filtrate
by filtering it using filter paper, then the precipitate is washed using aquades
with the aim that there is no filtrate left in the precipitate and to remove
excess when added HCl 6M and diluted HCl in the initial step. Basically, the
deposits formed are cations from group I, while the filtrates are groups II, III,
IV, and V.
After the precipitate is washed, the next process is that the precipitate
is heated in a water bath ±1 minutes and produces a clear solution and a
white precipitate that was originally cloudy white. The purpose of this heating
process is to separate Pb from Ag and Hg by dissolving Pb. Because basically
Pb is easily soluble at high temperatures and when cold will crystallize again
forming a needle. Furthermore, the heated solution was centrifuge for ±2
minutes to produce a white precipitate and colorless filtrate and the
precipitate was filtered using filter paper and washed using aquades. The
filtrate produced from this centrifuge process is a Pb2+ filtrate. To prove the
presence or absence of Pb2+ cations in the filtrate, treatment is carried out by
 adding 2 drops of CH3COOH solution with the aim of precipitating Pb,
because Pb is a metal that dissolves even in weak acids. After that, 1 drop of
K2CrO4 solution is added with the aim of giving a yellow color to the
precipitate formed if the filtrate contains cations Pb2+. In the experiments
that have been carried out, it was found that there was a yellow precipitate
in the CD sample solution added K2CrO4 solution which showed that CD
sample solutions contain Pb2+ cations.
The next process is to add 0.5 ml of NH4OH solution to the precipitate
that has been formed earlier. The purpose of adding NH4OH is to separate Ag
from Hg where Ag will dissolve in NH4OH while Hg will form a precipitate.
NH4OH itself is NH3 that ionizes when dissolved in water. Then after the
addition of NH4OH, the solution is stirred, heated, and centrifuge to produce a
colorless filtrate and a black precipitate of Hg (NH2)Cl and Hg if the
precipitate contains cations Hg22+. However, based on experiments that
have been carried out, CD and BE sample solutions do not form black
deposits so that it can be interpreted that the sample solution does not
contain cations Hg22+. Furthermore, the resulting filtrate is added with dilute
HCl with the aim of precipitating group I cations, especially Ag, if a white
precipitate is formed, the filtrate it contains Ag+ cations. Based on
experiments that have been done, in the BE sample solution a white
precipitate is formed after adding diluted HCl, it shows that the solution BE
samples contain Ag+ cations.
b. Anion Analysis
In the second experiment, analysis of nitrate anions (NO3-), sulfate
(SO42-), and chloride (Cl-) was carried out in 2 sample solutions that had been
given, namely sample solutions CD and BE sample solution. The first step is
to make a preparation solution by adding Na2CO3 solution to the sample
solution and then heated. The purpose of adding Na2CO3 is to separate cations
and anions where cations or carbonate salts will precipitate while anions or
sodium salts will dissolve in sample solution. Further solutions of Na2CO3
in the precipitation reaction can be replaced with sulfates, peroxidesulfates,
phosphates, phosphites, hypophosphites, arsenates, arsenites, chromates,
dichromate, silicate, hex fluorosilicate, salicylate, benzoate, and succinate.
While in redox reactions Na2CO3 can be replaced with manganate,
permanganate, chromate, and dichromate. The purpose of heating is that
carbonate salts contained in the solution will release CO2 and become metals so
that they can dissolve sodium salts that It is likely that it has not dissolved.
After heating, it is then separated between the precipitate and the filtrate by
filtering. The resulting filtrate acts as a preparation solution used to determine
nitrate anions.
After the preparation solution is complete, nitrate ion proof (NO3-) is
carried out by adding 8 drops of concentrated H2SO4 solution to the BE sample
solution and 14 drops to the CD sample solution. After the addition of
concentrated H2SO4 this nitrate gas is formed which is characterized by the
presence of gas bubbles and hot taste. This process is called the exothermic
process or heat transfer from the system to the environment. The next step to
prove the presence of nitrate ions is to slowly add FeSO4 to the sample
solution. In the BE sample solution 5 drops were added and 9 drops of CD
sample solution were added. If the sample solution contains nitrate ions , then
after the addition of FeSO4 this brown ring will form.
In the process of adding H2SO4 and FeSO4, H2SO4 can be added first or
FeSO4 first because for the brown ring test, it can be done in one of these two
ways: (a) Add 3 ml of the iron(II) sulfate solution just made to 2 ml of the nitrate
solution, and slowly pour 3-5 ml of concentrated sulfuric acid along the side of
the test-tube so that it forms a layer at the bottom of the mixture the. A brown
ring will form where the two liquids meet. (b) Slowly add 4 ml of concentrated
sulfuric acid to 2 ml of the nitrate solution, mix the liquids thoroughly, and cool
the mixture under running cold water from a tap. Slowly pour the saturated
solution of iron(II) sulfate down the side of the tube so that it forms a layer on
top of the liquid. A brown ring will form in the contact zone between the two
liquids. This brown ring is due to the formation of [Fe(NO)]2+. After the mixture
was shaken and heated, this brown color disappeared, nitrogen (II) oxide was
released. and a yellow solution of iron(III) ions remains. Based on the
experiments that have been carried out, it was found that there are brown rings
in both sample solutions, namely CD and BE sample solutions. Where it shows
both sample solutions contain nitrate ions.
The next process is to test the sulfate ions on both sample solutions. The
first step is to add HCl 6M to the CD and BE preparation solution. The purpose
of adding HCl 6M is to acidify the sample solution, so that minerals can
dissolve. In CD preparation solution, the addition of HCl and boiling causes a
clear solution while in BE preparation solution, the addition of HCl 6M and
boiling causes a cloudy white solution. Furthermore, both preparation solutions
are added with BaCl2 solution with the aim that the sulfate can be bound by
Ba ions, thus forming a white precipitate, namely BeSO4. A solution is said to
contain sulfate anions if a white precipitate forms after the addition of BaCl2.
And based on experiments that have been done, the CD sample solution does
not form a white precipitate which means that the CD sample solution does
not contain sulfate ions, while in the BE sample solution a white precipitate
is formed after the addition of BaCl2. This shows that both sample solutions
contain sulfate ions.
The last process is testing chloride ions on both sample solutions. The
first step is to add AgNO3 solution to the CD and BE preparation solution.
The purpose of adding AgNO3 solution is to precipitate Cl- as AgCl. The
precipitate can be formed because the solubility product of the solution has
been exceeded by the product of the concentration of the ions involved, or it
can be written Qc>Ksp. In the CD sample solution after the addition of
AgNO3 the solution is clear and a turbid white precipitate is formed, while in
the BE preparation solution, the solution is clear and a white precipitate
is formed . The next step is to add NH4OH solution to the CD and BE
preparation solution. The function of adding NH4OH solution is to dissolve
AgCl. Based on the experiments that have been carried out, both sample
solutions, namely CD and BE, both form a turbid white precipitate after the
addition of NH4 OH. This shows that both sample solutions do not contain
chloride ions. While based on theory, CD sample solutions contain chloride
ions.
X. Discussion
In this second experiment, no Cl- anion was found in the CD sample.
This happens because it can be caused by the lack of addition of NH4OH to
dissolve AgCl deposits, and AgCl deposits in our group are too much so that
the volume of addition of NH4OH is less to dissolve AgCl precipitates. And
we don't wait for the precipitate to dissolve or not, so we still get an
insoluble precipitate and immediately conclude that there is no soluble
precipitate.

XI. Conclusion
Based on the results of observations that have been made, it can be
concluded that :
1) In the group 1 cation analysis experiment, sample BE solution doesn’t
contain Pb2+ and Hg22+, but contain Ag+. This characterized by the presence
of a white precipitate. While for sample CD solution doesn’t contain Hg22+
and Ag+, but contain Pb2+. This characterized by the presence of a yellow
precipitates.
2) In the anion proof experiment (sulfate ion, chloride ion and nitrate ion),
sample BE solution contain SO42- as seen presence of a white precipitate
and contain NO3- as seen presence of a brown ring. While for sample CD
solution just contain NO3- as seen by the presence of a brown ring.

XII. Suggestion
1) Before doing the practicum, you should pray so that the practicum runs
smoothly as you wish.
2) Before doing the practicum, you should understand every step that will be
carried out during the practicum.
3) Before doing the practicum, you should understand the use of tools and
materials and how to use them.
4) When doing practicum should be more careful so as not to make mistakes.
XIII. References

Alhasan, H. S., & Alahmadi, N. (2021). Principles of Qualitative Inorganic

Analysis: Precipitation, Separation and Identification of Cations. Bentham
Science Publishers.

Kunsah, B., Kartikorini, N., Mardiyah, S., & Ariana, D. (2019). Modul Praktikum
Kimia Analitik Kualitatif.

Muntean, E. (2022). Food Analysis: Using Ion Chromatography. Walter de

Gruyter GmbH & Co KG.

Roy, P. S. (2021). A Guidebook to Qualitative Inorganic Analysis. A Guidebook

to Qualitative Inorganic Analysis, 1-19.

XIV. Attachment
a. Answer Questions
1) Write the general reaction for each group!
(Group I : M+ + Cl- → MCl(s) (white)
Answer :
Group I
- Pb2+ + CrO42- → PbCrO4 ↓ (yellow precipitate)
- Hg2Cl2 + 2NH3 → Hg ↓ + Hg(NH3)2Cl ↓ + NH4+ + Cl- (black precipitate)
- [Ag(NH3)2]+ + Cl- → AgCl + NH4+ (white precipitate)
Group IIA
- Hg2+ + S2- → HgS ↓
- Pb2+ + S2- → PbS ↓
- Bi3+ + S2- → Bi2S3 ↓
- Cu2+ + S2- → CuS ↓
- Cd2+ + S2- → CdS ↓
- As3+ + S2- → As2S3 ↓
- Sb3+ + S2- → Sb2S3 ↓
- Sn2+ + S2- → SnS ↓
Group IIB
- Hg2+ + S2- → HgS ↓
- As3+ + S2- → As2S3 ↓
- Sb3+ + S2- → Sb2S3 ↓
- Sn2+ + S2- → SnS ↓
Group IIIA
- Fe2+ + 2OH- → Fe(OH)2 ↓
Group IIIB
- Mn2+ + S2- → MnS ↓
Group IV
- Ba2+ + CO32- → BaCO3 ↓
- Ba2+ + CrO42- → BaCrO4 ↓
- Sr2+ + CO32- → SrCO3 ↓
- Sr2+ + CrO42- → SrCrO4 ↓
- Ca2+ + CO32- → CaCO3 ↓
- Ca2+ + CrO42- → CaCrO4 ↓
- Ca2+ + (-COOH)22- → Ca(COOH)2 ↓
Group V
- Mg2+ + 2OH- → Mg(OH)2 ↓
2) Why is the oxidizing agent used in the cationic analysis of the H2S system
H2O2 or naair bromine, and not HNO3?
Answer:
In the cation analysis using the H2S system, the oxidizing agent H2O2 or
bromine water is used because H2O2 or bromine water easily evaporates
when added to water so that a precipitate of sulfide salts is obtained from
H2S. If you use HNO3 as an oxidizing agent, no precipitate of sulfide salts
will form because H2S is flowed into the analyte in an acidic
environment, whereas if you use an oxidizing agent, HNO3, all the acid
must be removed.
1) How do you know if H2S, H2O2, or Br2 is no longer in solution?
Answer:
a) To find out that H2S was not present in the solution, Pb-acetate paper
was replaced.
 b) To find out that H2O2 is not present in the solution, by dipping the filter
paper into HCl. Then attached to the hose hole that is channeled to
H2O2. If there are no black stains on the filter paper, then H2O2 is no
longer in solution.
c) To find out that Br2 is no longer in the solution, by evaporating the
solution. Then the smoke that comes out is placed on the wet starch
paper. If the paper turns orange red then Br2 is still present and if the
paper is orange then Br2 is not in solution.
2) Why does the analyte have to be used to determine the presence of NH4+
cations directly?
Answer:
Because in the group IV filtrate there is already a cation NH4+ added to
the process of separating groups I, II, III. So to determine the presence of
NH4+ cations, you have to use the analytes directly.
3) What is the reaction in general when preparing a preparatory solution to
determine the presence of anions?
Answer:
MA2+ + Na2CO3 ⇄ MCO3 + 2NaA
4) The precipitation of sulfide salts in the analysis of group II and group IIIB
cations was carried out in different aqueous conditions. Explain!
Answer:
a) In group II, H2S flows into an acidic solution because the filtrate is
used to get the precipitate the sulfide salt comes from group I filtrate
which still contains dilute HCl.
b) In group IIIB the solution is alkaline, because the filtrate used to
precipitate the sulfide salt comes from group IIIA filtrate which still
contains NH3 and NH4Cl.

7) Why does group IV deposition have to be in an alkaline environment?

Answer:

Because in the group IV precipitation process, the NH4OH solution added

before the filtrate is heated can prevent the loss of volatile acids so that it will
 produce carbonate salts derived from ammonium carbonate. So that the
deposition of group IV must be in alkaline conditions.

b. Documentation
1. Cation Analysis
a) Sample Y (CD)

No Gambar Keterangan

Added the y sample to the

1. reaction tube

2. Added with few drops of 6M HCl

3. Added with 1 to 2 drops of diluted

HCl
4. Centrifuged

Precipitates and Filtrate are created

5-. by the Centrifuges process

Filtrate and precipitates are filtered

6. using filter paper

Pb+ filtrates added with 2 drops of

7. CH3COOH solution
 Then added with few drops of
8. K2CrO4 solution

Yellow precipitates of PbCr

9.

Precipitate dissolved with 0,5mL

10. NH4OH 6M

11. Heated on hot water bath

12. Centrifuged for 1 minutes

Filtered the filtrates and precipitate

13.

Added HCl to the filtrate

14.

White precipitates of ag doesn’t

15. appeared
b) Sample X (BE)
No Gambar Keterangan

Added the x sample to the

1. reaction tube

2. Added with few drops of 6M HCl

3. Added with 1 to 2 drops of diluted

HCl

4. Centrifuged
 Precipitates and Filtrate are created
5-. by the Centrifuges process

Filtrate and precipitates are filtered

6. using filter paper

filtrates added with 2 drops of

7. CH3COOH solution

Then added with few drops of

8. K2CrO4 solution
 Yellow precipitates of PbCr
9.

Precipitate dissolved with 0,5mL

10. NH4OH 6M

11. Heated on hot water bath

12. Centrifuged for 1 minutes

 Filtered the filtrates and precipitate
13.

Added HCl to the filtrate

14.

White precipitates of ag doesn’t

15. formed instantly but will appear
after some time
2. Anion Analysis

a) Sample X (BE)
✓ Proof of chloride ion (Cl-)

No. Picture Information

1. Added sample X with
saturated Na2CO3

2. Heated sample X which

has been added saturated
Na2CO3

3. Filtered the precipitate

4. Added AgNO3 solution

5. Added NH4OH solution

✓ Proof of sulfate ion (SO42-)

No. Picture Information

1. Added sample X with
saturated Na2CO3

2. Heated sample X which

has been added saturated
Na2CO3

3. Filtered the precipitate

4. Added sample X with
6M HCl until sour

5. Brought to a boil

6. Added BaCl2 solution

✓ Proof of nitrate ion (NO3-)

No. Picture Information

1. Added sample X with
saturated Na2CO3
2. Heated sample X which
has been added saturated
Na2CO3

3. Filtered the precipitate

4. Added concentrated
H2SO4

5. Added saturated FeSO4

solution
 b) Sample Y (CD)
✓ Proof of chloride ion (Cl-)

No. Picture Information

1. Added sample Y with
saturated Na2CO3

2. Heated sample Y which

has been added saturated
Na2CO3

3. Filtered the precipitate

4. Added AgNO3 solution

5. Added NH4OH solution

✓ Proof of sulfate ion (SO42-)

No. Picture Information

1. Added sample Y with
saturated Na2CO3

2. Heated sample Y which

has been added saturated
Na2CO3

3. Filtered the precipitate

4. Added sample Y with
6M HCl until sour

5. Brought to a boil

6. Added BaCl2 solution

✓ Proof of nitrate ion (NO3-)

No. Picture Information

1. Added sample Y with
saturated Na2CO3
2. Heated sample Y which
has been added saturated
Na2CO3

3. Filtered the precipitate

4. Added concentrated
H2SO4

5. Added saturated FeSO4

solution